STUDY OF HALOGENATED HYDROXYPHENAZINES

1957 ◽  
Vol 35 (12) ◽  
pp. 1423-1433 ◽  
Author(s):  
Paul E. Gagnon ◽  
Karl F. Keirstead ◽  
Brian T. Newbold
Keyword(s):  
Hydrogen Peroxide ◽  
Molecular Weight ◽  
Thermal Decomposition ◽  
Acetic Acid ◽  
Absorption Spectra ◽  
Glacial Acetic Acid ◽  
Zinc Dust ◽  
Sodium Perborate ◽  
Chemical Evidence

The properties of chlorotrihydroxydihydrophenazine were thoroughly investigated. Oxidations with sodium perborate or hydrogen peroxide in glacial acetic acid gave chloro-trihydroxyphenazine-5,10-dioxide. Methylation gave a monomethyl derivative and acetylation yielded mono-, di-, and tri-acetyl derivatives. Benzoylation gave a tetrabenzoyl compound. Bromination gave a monobromo derivative. Nitrosation produced a mononitroso and nitration a mononitro compound. Degradation by zinc dust distillation and thermal decomposition yielded phenazine. Molecular weight and absorption spectra determinations supported the chemical evidence that the compound was 1-chloro-2(or 3),6,8-trihydroxydihydrophenazine. 1,4,9-Trichloro-2(or 3),6,8-trihydroxydihydrophenazine, 1,4,9-trichloro-2(or 3, or 8),6-dihy-droxydihydrophenazine, and 1-bromo-2(or 3),6,8-trihydroxydihydrophenazine were similarly identified.

Preparations, sulphinate coordination, and thermal decomposition of some bismuth triarenesulphinates

1972 ◽  
Vol 25 (10) ◽  
pp. 2107 ◽  
Author(s):  
GB Deacon ◽  
GD Fallon
Keyword(s):  
Thermal Decomposition ◽  
Acetic Acid ◽  
Sulphur Dioxide ◽  
Glacial Acetic Acid ◽  
The Other

Bismuth triarenesulphinates, Bi(02SR)3 [R = Ph, p-MeC6H4, p-ClC6H4, 2,4,6-(Me2CH)3C6H2, and p-MeCONHC6H4], have been prepared by reaction of bismuth triacetate with the appropriate arenesulphinio acids in glacial acetic acid, and the first two compounds have also been obtained by reaction of triphenyl-bismuth with the appropriate mercuric arenesulphinates. The sulphur-oxygen stretching frequencies of the bismuth sulphinates are indicative of O-sulphinate coordination, and the compounds are considered to be polymeric with bridging O-sulphinate groups and six-coordinate bismuth. Thermal decomposition of Bi(O2SR)3 (R = Ph, p-MeC6H4, or p-CIC6H4) under vacuum gave the corresponding triarylbismuth compounds and sulphur dioxide, the preparation of tri-p-chlorophenylbismuth being accompanied by formation of di-p-chlorophenyl sulphone and S-p-chlorophenyl p-chlorobenzenethiosulphonate. Pyrolysis of the other triarenesulphinates did not yield organobismuth compounds.

A new method for the preparation of peroxymonophosphoric acid

2003 ◽  
Vol 81 (2) ◽  
pp. 156-160 ◽  
Author(s):  
Tian Zhu ◽  
Hou-min Chang ◽  
John F Kadla
Keyword(s):  
Hydrogen Peroxide ◽  
Acetic Acid ◽  
Carbon Tetrachloride ◽  
Glacial Acetic Acid ◽  
Acid Synthesis ◽  
Conversion Ratio ◽  
New Method ◽  
Phosphorous Pentoxide ◽  
Preparation Conditions ◽  
Peroxy Acids

A new method for the preparation of peroxymonophosphoric acid (H3PO5) has been developed. It utilizes a biphasic solution to moderate the vigorous reaction between phosphorous pentoxide (P2O5) and hydrogen peroxide (H2O2). P2O5 is suspended in carbon tetrachloride (CCl4), and concentrated H2O2 is slowly added while being vigorously stirred at low temperature. Careful control of the reaction temperature through the slow addition of H2O2 is critical. Using typical preparation conditions (P2O5:H2O2 = 0.5:1, H2O2 70 wt %, 2°C, 120–180 min), ~70% of the H2O2 is effectively converted to H3PO5. Increasing the concentration of H2O2, as well as the mole ratio of P2O5:H2O2, leads to an even higher % conversion of H2O2 to H3PO5. The addition of glacial acetic acid to the P2O5:H2O2 suspension at the end of the 120–180 min reaction (P2O5:H2O2:CH3COOH = 0.5:1:0.3) leads to the formation of peracetic acid in addition to H3PO5, and to an overall increase in the conversion ratio of total peroxy acids based on H2O2 (>95%).Key words: peroxymonophosphoric acid, synthesis, stability, conversion ratio.

scholarly journals Synergistic Extraction and Characterization of Fulvic Acid by Microwave and Hydrogen Peroxide–Glacial Acetic Acid to Oxidize Low-Rank Lignite

ACS Omega ◽  
2020 ◽  
Vol 5 (12) ◽  
pp. 6389-6394
Author(s):  
Yingjie Zhang ◽  
Guanqun Gong ◽  
Honglei Zheng ◽  
Xin Yuan ◽  
Liangwei Xu
Keyword(s):  
Hydrogen Peroxide ◽  
Acetic Acid ◽  
Fulvic Acid ◽  
Glacial Acetic Acid ◽  
Synergistic Extraction ◽  
Low Rank

scholarly journals PERACETIC ACID OXIDATION OF HALOGENATED AZOBENZENES

1959 ◽  
Vol 37 (2) ◽  
pp. 366-369 ◽  
Author(s):  
Paul E. Gagnon ◽  
Brian T. Newbold
Keyword(s):  
Hydrogen Peroxide ◽  
Acetic Acid ◽  
Peracetic Acid ◽  
Glacial Acetic Acid ◽  
Acid Oxidation ◽  
Azoxy Compounds

A series of dihalogenated and five tetrachloroazobenzenes were oxidized to the corresponding azoxy compounds by means of 30% hydrogen peroxide in glacial acetic acid, the reaction being carried out at about 60–70 °C, for 24 hoursAs expected, the yields, in general, obtained from azobenzenes containing substituents in the 2,2′-positions were lower than those from compounds having substituents in the 3,3′- and 4,4′-positions, which gave very good results.

scholarly journals Synthesis of Bioactive Fluorinated 10H-Phenothiazines and their Sulfone Derivatives

2008 ◽  
Vol 5 (s1) ◽  
pp. 1063-1068 ◽  
Author(s):  
Yogesh Dixit ◽  
Rahul Dixit ◽  
Naveen Gautam ◽  
D. C. Gautam
Keyword(s):  
Hydrogen Peroxide ◽  
Acetic Acid ◽  
Spectroscopic Data ◽  
Halogen Atom ◽  
Glacial Acetic Acid ◽  
Present Communication ◽  
Smiles Rearrangement ◽  
Antimicrobial Studies ◽  
Sulfone Derivatives

The present communication deals with the synthesis of a series of fluorinated 10H-phenothiazines. 10H-phenothiazines is prepared by Smiles rearrangement of substituted 2-foramido-2´-nitrodiphenylsulfide. Substituted 2-foramido-2´-nitrodiphenylsulfide were obtained by the reaction of 2-amino-3-fluorobenzenethiol witho-halonitrobenzenes followed by formylation and 1-nitro/1-halo-10H-phenothiazines have been prepared by the reaction of substituted 2-aminobenzenethiols with reactiveo-halonitrobenzene containing a nitro group or halogen atom ato-position to the reactive halogen atom directly yielded 1-nitro/1-halo-10H-phenothiazines in situ. 10H-phenothiazine sulfone derivatives have been synthesized by the oxidation of 10H-phenothiazines by 30% hydrogen peroxide in glacial acetic acid. The structure of the synthesized compounds has been characterized by spectroscopic data and elemental analysis. Antimicrobial studies of the synthesized compounds have also been included.

Response Surface Methodology for Optimization of Epoxidized Trimethylolpropane Ester Synthesis from Palm Oil

2011 ◽  
Vol 9 (1) ◽  
Author(s):  
Ferra Naidir ◽  
Robiah Yunus ◽  
Irmawati Ramli ◽  
Tinia I. Mohd. Ghazi
Keyword(s):  
Hydrogen Peroxide ◽  
Response Surface Methodology ◽  
Acetic Acid ◽  
Regression Model ◽  
Palm Oil ◽  
Iodine Value ◽  
Glacial Acetic Acid ◽  
Oxirane Oxygen ◽  
Dependent Variables

To improve the oxidative stability of the palm oil-based biolubricant, the fatty acid double bonds in palm oil-based trimethylolpropane ester (TMP ester) was converted into an oxirane ring via an in-situ epoxidation method. The epoxidized TMP ester was produced from a reaction between TMP ester and peracetic acid which was prepared in-situ by reacting glacial acetic acid with hydrogen peroxide in the presence of concentrated sulphuric acid. The response surface methodology was applied using a central composite design technique to optimize the conditions of the epoxidation reaction to produce the epoxidized TMP ester. The effects of four independent variables namely concentration of acetic acid (0-2 mol), concentration of hydrogen peroxide (1.5-9.5 mol), temperature of reaction (30-110°C) and reaction time (0.5-26.5 h) on the three dependent variables; percentage of oxirane oxygen, iodine value, and hydroxyl value were studied. A second-order polynomial multiple regression model was employed to predict the three dependent variables under optimum conditions of 0.59 mol of glacial acetic acid, 7.5 mol of hydrogen peroxide concentration, at temperature of 50°C and reaction times of 7 h. The optimum values of percentage of oxirane oxygen, iodine value, and hydroxyl value were 4.01%, 1.94%, and 0.43% respectively. The analysis of variance yielded a high coefficient of determination value of 0.9395-0.9880, hence indicating the fitness of the second-order regression model to the experimental data.

scholarly journals Synthesis of Epoxidizedcardanol from CNSL Vietnam by Glacial Acetic Acid and Hydrogen Peroxide

2017 ◽  
Vol Volume-1 (Issue-6) ◽  
pp. 1271-1275
Author(s):  
Bach Trong Phuc ◽  
Vu Van Hai ◽  
Nguyen Thi Hien | Nguyen Thanh Liem ◽  
Keyword(s):  
Hydrogen Peroxide ◽  
Acetic Acid ◽  
Glacial Acetic Acid

THE BROMINOLYSIS OF CARBOHYDRATE IODIDES: I. ACETYLATED 6-DEOXY-6-IODO AND 2-DEOXY-2-IODO GLYCOSIDES

1964 ◽  
Vol 42 (3) ◽  
pp. 539-546 ◽  
Author(s):  
R. U. Lemieux ◽  
B. Fraser-Reid
Keyword(s):  
Acetic Acid ◽  
Methoxy Group ◽  
Glacial Acetic Acid ◽  
Main Product ◽  
Zinc Dust ◽  
Potassium Acetate ◽  
Borohydride Reduction ◽  
Silver Acetate ◽  
Sodium Borohydride Reduction ◽  
Dust Reduction

Reaction of methyl 6-deoxy-6-iodo-α-D-glucopyranoside triacetate with an excess of bromine in glacial acetic acid; N in potassium acetate, gave a 1.1:1 mixture of the products resulting from replacement of the iodine by bromine and by acetoxy group, respectively. When 2 moles of silver acetate were present per mole of bromine, the reaction was much more rapid and only methyl α-D-glucopyranoside tetraacetate was formed. The brominolysis of methyl 2-deoxy-2-iodo-α-D-mannopyranoside triacetate proceeded at a useful rate only when catalyzed by silver acetate. The main product of the reaction appeared to be methyl 3-acetoxy-2-bromo-2-deoxy-α-D-arabino-hexopyranoside triacetate. The compound could be converted by way of sodium borohydride reduction to methyl 2-bromo-2-deoxy-α-D-altropyranoside and by way of zinc dust reduction to methyl 2-deoxy-α-D-erythro-hexopyranoside-3-ulose diacetate. About 20% of the reaction proceeded with migration of the methoxy group to the 2-position to yield 2-O-methyl-D-glucose tetraacetate. The mechanisms of these reactions are discussed.

scholarly journals Study on the Factors Influencing the Extraction of Chenodeoxycholic Acid from Duck Bile Paste by Calcium Salt Method

2018 ◽  
Vol 2018 ◽  
pp. 1-6 ◽  
Author(s):  
Xiangzheng Hu ◽  
Na Feng ◽  
Jiaqi Zhang
Keyword(s):  
Hydrogen Peroxide ◽  
Acetic Acid ◽  
Calcium Chloride ◽  
Methyl Alcohol ◽  
Chenodeoxycholic Acid ◽  
Glacial Acetic Acid ◽  
Calcium Salt ◽  
Orthogonal Experimental Design ◽  
Optimum Conditions ◽  
Extraction Technology

New extraction technology of chenodeoxycholic acid from duck bile paste by calcium salt was investigated. The optimum conditions of extraction were determined by orthogonal experimental design. The results indicated that influencing factors on the extraction efficiency of chenodeoxycholic acid were as follows: hydrogen peroxide, methyl alcohol, glacial acetic acid, and calcium chloride. The optimum extracting conditions of chenodeoxycholic acid were 1000 mL amount of methyl alcohol, 50 mL amount of hydrogen peroxide, 500 mL amount of 20% calcium chloride, and 600 mL amount of 60% glacial acetic acid for a quantity of duck paste. The yield of chenodeoxycholic acid was 30%.

ChemInform Abstract: Considered as Synthetic Methods and Reaction. Part 175. Convenient Oxidation of Oximes to Nitro Compounds with Sodium Perborate in Glacial Acetic Acid.

ChemInform ◽  
2010 ◽  
Vol 23 (39) ◽  
pp. no-no
Author(s):  
G. A. OLAH ◽  
P. RAMAIAH ◽  
C.-S. LEE ◽  
K. S. PRAKASH G
Keyword(s):  
Acetic Acid ◽  
Glacial Acetic Acid ◽  
Nitro Compounds ◽  
Synthetic Methods ◽  
Sodium Perborate
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