scholarly journals Chlorocruoroporphyrin: a Simple Method of Preparation

1953 ◽  
Vol 32 (2) ◽  
pp. 365-366 ◽  
Author(s):  
Gilbert Y. Kennedy
Keyword(s):  
Acetic Acid ◽  
Hydrazine Hydrate ◽  
Potassium Permanganate ◽  
Sodium Acetate ◽  
Glacial Acetic Acid ◽  
Small Sample ◽  
Mixed Crystals ◽  
Distilled Water ◽  
Simple Method ◽  
Marine Polychaete

Munro Fox (1926, Addendum, p. 219) described a method of preparation of chlorocruoroporphyrin from the blood of the marine polychaete worm Spirographis. This was based upon the very troublesome method of Nencki & Zaleski (1900), which is time-consuming and wasteful. Furthermore, Spirographis is not easily obtainable in this country. Lemberg & Parker (1952) started with protoporphyrin, and by careful oxidation with potassium permanganate in acetone obtained a solution which gaVe mixed crystals of chlorocruoroporphyrin and diformyldeuteroporphyrin esters. Purification was by fractional chromatography. The procedure to be described here is simple and rapid, and could easily be carried out in one day by a biologist requiring a small sample of the porphyrin. The two methods mentioned above would not come into this category.This work was done at the Plymouth Laboratory, and I am very grateful to Mr T. R. Tozer of that laboratory for so kindly obtaining the animals for me and extracting the blood.The polychaete worms Myxicola infundibulum, Sabella pavonina and Branchiomma vesiculosum are all readily obtained from the muddy shores of the Salcombe estuary, especially on the Salstone. Blood was taken directly from the vessels of about 100 assorted worms by syringe, and squirted as it was removed from the worms into a mixture of peroxide-free ether (3 parts) and ‘Analar’ glacial acetic acid (1 part). After all the blood had been added, the mixture was well shaken and allowed to stand in the ice-chest for 30 min. The acetic acid was then washed out with distilled water, the first few washings containing a little sodium acetate to avoid washing out of the pigment, and the remaining solution of chlorocruorohaematin dried roughly by filtering through ether-soaked paper into a distilling flask and evaporated to dryness. 100 ml. of a 50% solution of hydrazine hydrate in glacial acetic acid were then added, and the mixture heated on a water-bath at 90° C. for 10 min.

Synthesis and Caracterization of some New 1H-3-aryl-7-etoxycarbonyl-6-methyl-pyrazolo[5,1-c][1,2,4]triazoles

2008 ◽  
Vol 59 (1) ◽  
pp. 41-44
Author(s):  
Maria-Daniela Sofei ◽  
Maria Ilici ◽  
Valentin Badea ◽  
Carol Csunderlik ◽  
Vasile-Nicolae Bercean
Keyword(s):  
Mass Spectrometry ◽  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Sodium Acetate ◽  
Glacial Acetic Acid ◽  
Ir And Nmr Spectroscopy

The synthesis of 1H-3-aryl-7-ethoxycarbonyl-6-methyl-pyrazolo[5,1-c][1,2,4]triazoles (2) was carried out by cyclization of 1H-5-arylidenehydrazino-4-ethoxycarbonyl-3-methyl-pyrazoles (1) in the presence of bromine using glacial acetic acid as solvent and sodium acetate as base. The new nine obtained compounds were characterized by IR and NMR spectroscopy and mass spectrometry.

STUDIES ON THE FORMATION OF HEXAMINE

1952 ◽  
Vol 30 (9) ◽  
pp. 687-693 ◽  
Author(s):  
T. R. Ingraham ◽  
C. A. Winkler
Keyword(s):  
Activation Energy ◽  
Acetic Acid ◽  
Acid Solution ◽  
Induction Period ◽  
Ammonium Nitrate ◽  
Sodium Acetate ◽  
Glacial Acetic Acid ◽  
Initial Rate ◽  
Acetic Acid Solution ◽  
Rate Data

Rate curves have been determined for the reaction of ammonium nitrate with formaldehyde in glacial acetic acid solution at 25 °C., 35 °C., 45 °C., and 55 °C. over a range of Initial mole ratios (formaldehyde: ammonia) of 0.75:1 to 9.0:1. Data obtained at 25 °C. show a definite induction period in the formation of hexamine. The length of the induction period is not changed by increasing ammonium nitrate concentrations above the theoretical (1.5:1), but may be appreciably shortened by initial additions of excess formaldehyde or of sodium acetate. From 35 °C. upward, the induction period is not apparent. The order of the reaction with respect to formaldehyde has been determined from initial rate data, and an activation energy calculated. The reactions in general appear analogous to those found in slightly acid aqueous systems.

THE PREPARATION OF 9-HYDROXYPYRAZOLO[3,4-b]QUINOLINES

1966 ◽  
Vol 44 (17) ◽  
pp. 2009-2014 ◽  
Author(s):  
R. T. Coutts ◽  
J. B. Edwards
Keyword(s):  
Acetic Acid ◽  
Acetic Anhydride ◽  
Hydrazine Hydrate ◽  
Sodium Borohydride ◽  
Sodium Acetate ◽  
The Other ◽  
Reduction Product ◽  
Type I

4-(2-Nitrobenzylidene)-2-pyrazolin-5-ones (I) were best prepared by heating o-nitrobenzaldehyde and 2-pyrazolin-5-ones in acetic anhydride containing fused sodium acetate (cf. Erlenmeyer azlactone synthesis). Pyrazolones of type I were reductively cyclized with cyclohexene and palladium–charcoal, and gave 3a,4,9,9a-tetrahydro-9-hydroxy-1H-pyrazolo-[3,4-b]quinolines (II) which, as expected, were amphoteric compounds. Of the three other methods of reduction used in this study, two (zinc and acetic acid; sodium borohydride and palladium–charcoal) were capable of producing pyrazoloquinolines, but were less reliable. The other method employed (hydrazine hydrate and palladium–charcoal) caused degradation of the pyrazolone molecule in the two cases examined, and in both, bis(2-aminobenzylidene) hydrazine (V) was the reduction product isolated.

Condensation of Schiff bases with 2-oxazolin-5-ones: simultaneous introduction of arylidene and amino moieties

1982 ◽  
Vol 60 (3) ◽  
pp. 317-322 ◽  
Author(s):  
Arya K. Mukerjee ◽  
Pradeep Kumar
Keyword(s):  
Acetic Acid ◽  
Schiff Bases ◽  
Sodium Acetate ◽  
Glacial Acetic Acid ◽  
Methyl Group

Schiff bases condense with 2-oxazolin-5-ones having a C-4 methylene and/or C-2 methyl group, and the reaction in glacial acetic acid, containing freshly fused sodium acetate, produces 4-arylidene- and/or 2-styryl-2-imidazoline-5-ones as a result of simultaneous introduction of arylidene and amino moieties.

scholarly journals PEMBUATAN SELULOSA ASETAT DARI α -SELULOSA TANDAN KOSONG KELAPA SAWIT

2013 ◽  
Vol 2 (3) ◽  
pp. 33-39 ◽  
Author(s):  
M Roganda L Lumban Gaol ◽  
Roganda Sitorus ◽  
Yanthi S ◽  
Indra Surya ◽  
Renita Manurung
Keyword(s):  
Acetic Acid ◽  
Oil Palm ◽  
Sodium Acetate ◽  
Glacial Acetic Acid ◽  
Acid Anhydride ◽  
Ftir Analysis ◽  
Optimum Conditions ◽  
Empty Fruit Bunches ◽  
Last Stage ◽  
Cellulose Materials

Utilization of empty fruit bunches of oil palm in Indonesia is still very low, so it should be developed further. One of them by researching the manufacture of cellulose acetate from oil palm empty fruit bunches. The process used in this study is the cellanase with α-cellulose materials. Stages reaction is activation, acetylation, hydrolysis, neutralization and drying. Activation in thethree-neck flask with the addition of 50 ml of glacial acetic acid and stirredfor 3 hour,then added 15 ml of acetic acid anhydride as acetylation agent. Acetylation performed with the variation of time, 2, 2.5, 3, 3.5 hours.  In the hydrolysis step, add 2 ml of water and5 ml of glacial acetic acid. The reaction lasted for 30 minutes, then added 1 g of sodium acetate for neutralization, neutralization lasts for 5 minutes.  Then do the washing up to the smell of acetic acid is lost, and the last stage is the drying is done with a temperature below 50 oC.  The resulting products are then analyzed the degree of substitution, melting point, and then carried out FTIR analysis.  The results obtained when the optimum conditions for the acetylation reaction is 2.5 - 3 hours.

scholarly journals Synthesis and properties of 1-aminocarbonylmethyl-5-aryl- 4-aroyl-3-hydroxy-3-pyrroline-2-ones

2020 ◽  
Vol 64 (10) ◽  
pp. 28-32
Author(s):  
Vladimir L. Gein ◽  
◽  
Evgenia V. Pastukhova ◽  
Keyword(s):  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Physicochemical Properties ◽  
Hydrazine Hydrate ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Glacial Acetic Acid ◽  
Spectral Characteristics ◽  
Biologically Active ◽  
Three Component Reaction

3-Hydroxy-3-pyrrolin-2-ones are fully hydrogenated heterocyclic compounds, the base of which is included in a number of biologically active substances and drugs. Scientists' interest in 3-Hydroxy-3-pyrrolin-2-ones is due to the fact that, with their availability and high stability, they also have high reactivity due to the active carbonyl group in the third position of the heterocycle and easily interact with moconucleophiles. In addition, the presence of acyl and ethoxycarbonyl groups in the fourth position of the heterocycle makes it possible to obtain various condensed systems in reactions with binucleophiles, thereby making it possible to expand the range of the indicated compounds. We set the task to prepare 5-aryl-4-acyl-3-hydroxy-3-pyrrolin-2-ones containing an amino-carbonylmethyl substituent in the first position of the heterocycle, which were not previously described in the literature. It was also supposed to establish how the obtained compounds react with hydrazine hydrate. A series of 1-aminocarbonylmethyl-5-aryl-4-aroyl-3-hydroxy-3-pyrrolin-2-ones was obtained by setting up a three-component reaction of aroylpyruvic acid methyl ester with aromatic aldehydes and glycinamide hydrochloride in glacial acetic acid. The structure of the obtained compounds was established on the basis of IR and 1H NMR spectroscopy data. Based on the data of 1H NMR spectroscopy and a positive reaction with an alcoholic solution of iron(III) chloride, the predominant existence of the obtained compounds in the enol form was established. The article describes the mechanism of three-component reactions, the structural formulas of the obtained compounds, their physicochemical properties and spectral characteristics, as well as the yields of the reaction products. We have also studied the interaction of 1-substituted 5-aryl-4-acyl-3-hydroxy-3-pyrrolin- 2-ones with such a binucleophilic reagent as hydrazine hydrate. As a result of refluxing 1-amino-carbonylmethyl-3-hydroxy-4-(4-methoxybenzoyl)-5-(2-chlorophenyl)-3-pyrrolin-2-one and hydrazine hydrate in glacial acetic acid, 2-[4-(2-chlorophenyl)-3-(4-methoxyphenyl)-6-oxo-4,6-dihydropyrrolo [3,4-c] pyrazol-5(1H)-yl] acetamide. The article describes the proposed reaction mechanism, product yield, its physicochemical properties and spectral characteristics.

Novel Synthesis of 4-Aroyl-6-phenylpyridazin-3(2 H)-ones

1991 ◽  
Vol 46 (12) ◽  
pp. 1720-1722 ◽  
Author(s):  
M. F. Ismail ◽  
F. S. Sayed ◽  
S. A. Emara ◽  
A. A. Shindy
Keyword(s):  
Acetic Acid ◽  
Hydrazine Hydrate ◽  
Glacial Acetic Acid ◽  
Dimethyl Sulphate ◽  
Phosphorus Oxychloride ◽  
Hydroxylamine Hydrochloride ◽  
Sodium Dichromate ◽  
Novel Synthesis

4-Aroyl-6-phenylpyridazin-3(2 H)-ones (4a—c) were synthesized by the oxidation of the corresponding 4-arylmethyl-6-phenylpyridazin-3(2H)-ones (3a—c) using sodium dichromate in glacial acetic acid. The reactions of 4a—c with hydrazine hydrate and hydroxylamine hydrochloride proceeded smoothly to give the corresponding hydrazones (5) and oxime (6). 4a—c reacted with dimethyl sulphate to give 4-aroyl-2-methyl-6-phenylpyridazin-3(2 H)-ones (7a—c), respectively while their reaction with phosphorus oxychloride gave 4-aroyl-3-chloro-6-phenylpyridazines (9a—c), respectively.

A Simple Method to Prepare Affinity Resins on Cellulose Basis

1984 ◽  
Vol 39 (11-12) ◽  
pp. 1048-1051 ◽  
Author(s):  
Karl Eisele ◽  
Fernando Dias Costa ◽  
Carlos Pascual ◽  
Beatus Ofenloch-Hähnle
Keyword(s):  
Molecular Weight ◽  
Acetic Acid ◽  
Glacial Acetic Acid ◽  
Androgen Receptors ◽  
Methylene Chloride ◽  
Solid Phase ◽  
Solid Phase Peptide Synthesis ◽  
Low Molecular Weight ◽  
Amino Acid Residues ◽  
Simple Method

Abstract Affinity resins with different spacer arms were synthesized analogues to the solid phase peptide synthesis using aminoethyl cellulose or carboxymethyl cellulose as matrix. The spacer arms could be varied in length and rigidity. Especially spacer arms consisting of poly am ino acids can be synthesized with a defined amount of amino acid residues specifically in the low molecular weight ranges. The method is also applicable to other matrices w hich are not susceptible to 1 ɴ HCl in glacial acetic acid, trethylamine, methylene chloride and dimethylformamide. The synthesis of affinity resins with different spacer arms for the purification of androgen receptors is described as an example of the method.

scholarly journals SINTESIS DAN KARAKTERISASI SELULOSA ASETAT DARI ALFA SELULOSA TANDAN KOSONG KELAPA SAWIT

2018 ◽  
Vol 4 (1) ◽  
Author(s):  
M. Topan Darmawan ◽  
Muthia Elma ◽  
M. Ihsan
Keyword(s):  
Acetic Acid ◽  
Acetic Anhydride ◽  
Water Content ◽  
Cellulose Acetate ◽  
Sodium Acetate ◽  
Glacial Acetic Acid ◽  
Photographic Film ◽  
Ftir Analysis ◽  
Fiber Membrane ◽  
Acetyl Content

Selulosa asetat merupakan senyawa turunan selulosa yang sering digunakan sebagai serat, membran, dan film fotografi dalam industri. Tujuan dari penelitian ini adalah mengetahui pengaruh waktu asetilasi terhadap karakter selulosa asetat yang dihasilkan. Adapun proses yang digunakan dalam penelitian ini adalah proses cellanase dengan bahan baku tandan kosong kelapa sawit (TKKS). Tahapan reaksinya adalah aktivasi, asetilasi, dan hidrolisis. Aktivasi dilakukan di dalam labu leher tiga dengan penambahan asam asetat glacial 50 mL dan diaduk selama 3 jam pada kecepatan 125 rpm. Selanjutnya ditambahkan asetat anhidrida 15 mL sebagai agen asetilasi. Asetilasi dilakukan dengan variasi waktu, 2; 2,5; 3; dan 3,5 jam. Pada tahapan hidrolisis, ditambahkan air 2 mL dan asam asetat glacial 5 mL. Reaksi berlangsung selama 30 menit. Selanjutnya ditambahkan 1 gram natrium asetat untuk netralisasi yang berlangsung selama 5 menit. Kemudian dilakukan pencucian sampai bau asam asetat hilang. Tahapan terakhir adalah pengeringan yang dilakukan dengan suhu 55ºC selama 6 jam. Produk yang dihasilkan kemudian dianalisis kadar air, kadar asetil, rendemen dan gugus fungsi menggunakan analisa FTIR. Selulosa asetat yang terbaik diperoleh pada waktu asetilasi selama 2,5 jam dengan  kadar  asetil  40,36%, kadar  air  4.43%,  dan  rendemen 153,8%.Kata kunci: cellanase, selulosa, selulosa asetat. Cellulose acetate is a cellulose derivative which is often used as a fiber, membrane, and photographic film in industry. The  objectives  of  this  study  were  to determine the effect of acetylation time on the character of cellulose acetate. The process used in this study is the process of cellanase with α-cellulose of empty palm oil bunches materials. Stages of reaction are activation, acetylation, and hydrolysis. Activation was performed in a three-neck flask with the addition of 50 mL glacial acetic acid and stirred for 3 hours at 125 rpm. Then added 15 mL acetic anhydride as acetylation agent. Acetylation was performed by varying the time, 2; 2.5; 3; And 3.5 hours. At the hydrolysis stage, 2 mL of water and 5 mL glacial acetic acid were added. The reaction lasts for 30 minutes. Then added 1 gram of sodium acetate for neutralization lasts 5 minutes. then do the washing up to the smell of acetic acid disappeared. The final stage is the drying is done at a temperature of 55ºC for 6 hours. The resulting product was then analyzed for water content, acetyl content, rendement and functional groups using FTIR analysis. Cellulose acetate are best obtained at the time of acetylation for 2.5 hours with acetyl content of 40.36%, water content 4:43%, and a yield of 153.8%.Keywords: acetate cellulose, cellanase, cellulose.

Synthesis of Hexahydroindazole, Tetrahydro-[pyrimidoquinazolinone, benzodiisoxazolone] Derivatives and Anils from Diethyl 1,4-Cyclohexanedione-2,5-dicarboxylate

1980 ◽  
Vol 35 (10) ◽  
pp. 1310-1312 ◽  
Author(s):  
El-Sayed Afsah ◽  
Fathy A. Amer ◽  
Mohamed A. Metwally ◽  
Mohamed T. El-Zimaity
Keyword(s):  
Acetic Acid ◽  
Hydrazine Hydrate ◽  
Glacial Acetic Acid ◽  
The Other ◽  
Ethanolic Solution ◽  
Other Hand

Abstract Treatment of diethyl 1,4-cyclohexanedione-2,5-dicarboxylate (1) with hydrazine hydrate in glacial acetic acid afforded the diazobicycloocatdienedicarboxylate (2) and the azine (3). On the other hand, condensation of 1 with benzenesulphonylhydrazide in ethanolic solution gave the indazole derivative (4). Interaction of 1 with urea or hydroxyl-amine afforded the tetrahydropyrimidoquinazolinone (5) and the tetrahydrobenzodi-isoxazolone (6), respectively. Treatment of 1 with aniline gave the mono-anil (7) which, when subjected to Japp-Klingemann reaction with p-anisidine gave the dihydrazonoanil (8) and their condensation with benzidine in acetic acid gave the hydrazonoketoester (9). On the other hand condensation of 7 with hydrazine hydrate in ethanolic solution afforded the azobis (5-anilinoterephthalate) (10) and the hexahydrobenzodipyrazolone (11).

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