Synthesis of 7-hydroxy-4-methyl Coumarin with Microwave Radiation Catalyzed by Zirconium Sulfate Tetrahydrate

2013 ◽  
Vol 671-674 ◽  
pp. 2692-2696 ◽  
Author(s):  
Shu Jing Liu ◽  
Yun Peng Li ◽  
Xiu Min Yang ◽  
Qing Mei Jiang

The 1,3-benzenediol and ethyl acetoacetate as raw materials were used to synthesize 7-hydroxy-4-methyl coumarin under microwave irradiation with Zirconium sulfate tetrahydrate as the catalyst. The effect of various reaction conditionson on the yield was explored.Experiment shows that the yield reached up to 87. 5%,when the reaction conditions are as follow:n(1,3-benzenediol):n(ethyl acetoacetate)1.0, Zirconium sulfate tetrahydrate 0.4g,10mL cyclohexane, the reaction time 12 min,microwave radiation power 500W.

2019 ◽  
Vol 31 (5) ◽  
pp. 993-996 ◽  
Author(s):  
Sanjay S. Kotalwar ◽  
Amol D. Kale ◽  
Ram B. Kohire ◽  
Vasant B. Jagrut

An efficient and eco-friendly synthesis of 1,5-benzothiazepines has been developed by the reaction of various 2-propen-1-ones with 2-aminothiophenol using microwave irradiation in greener reaction medium, glycerol. The clean reaction conditions, shorter reaction time, high yields and non-toxic, biodegradable reaction medium manufactured from renewable sources are unique features of this method.


2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
Mantu Rajbangshi ◽  
Md. Rumum Rohman ◽  
Icydora Kharkongor ◽  
Hormi Mecadon ◽  
Bekington Myrboh

Iodine-alumina was employed as a catalyst in the coupling reactions of aldehydes, enolizable ketones, or 1,3-dicarbonyls with methyl carbamate or aromatic amines under microwave irradiation to afford β-amino carbonyl compounds in good-to-excellent yields. The key features of this environmentally friendly methodology are its operational simplicity, mild reaction conditions, and less reaction time.


2013 ◽  
Vol 781-784 ◽  
pp. 276-279
Author(s):  
Yu Hang Zhao ◽  
Li Cui ◽  
Da Zhi Wang ◽  
Tong Kuan Xu ◽  
Yong Peng Li

Butanone 1,2-propanediol ketal was synthesized by butanone and 1,2-propanediol as raw materials and sulfamic acid as catalyst. The effects of the mole ratio of raw materials agent, the dosage of the water-carrying agent and catalyst, reaction time on the product yield were discussed separately. Experimental results showed that sulfamic acid was a suitable catalyst for synthesizing of butanone 1,2-propanediol ketal. And the optimal reaction conditions are as follows: the mole ratio of butanone to 1,2-propanediol is 1:1.5, the amount of the catalyst is 2.2%, the water-carrying agent is 25ml, the reaction temperature is 358-378K and reaction time 3h. In this condition, the yield of production could reach 93.8%.


2021 ◽  
Vol 16 (9) ◽  
pp. 1934578X2110458
Author(s):  
Le Nhat Thuy Giang ◽  
Dang Thi Tuyet Anh ◽  
Hoang Thi Phuong ◽  
Nguyen Ha Thanh ◽  
Nguyen Thi Quynh Giang ◽  
...  

For the first time the 4-dimethylaminopyridine (DMAP) catalyzed straightforward and efficient procedure has been developed for the synthesis of 3,3′-(arylmethylene) bis(2-hydroxynaphthalene-1,4-dione) derivatives starting from lawsone (2-hydroxy-1,4-naphthoquinone) and a variety of (hetero)aromatic aldehydes in ethanol under microwave irradiation. Three of nine synthesized compounds are new. This method provides notable advantages over existing procedures including use of non-traditional basic catalyst and environmentally benign solvent, mild reaction conditions, excellent yields, short reaction time and simple workup.


2017 ◽  
Vol 5 (25) ◽  
pp. 6336-6342 ◽  
Author(s):  
Yan Sun ◽  
Jianli Wang ◽  
Mingzhe Chen ◽  
Chunsheng Li ◽  
Zhenpeng Hu ◽  
...  

The morphology-controlled preparation of t-Ba2V2O7 helical-like meso/nanosquares via a high-efficiency microwave radiation-assisted surfactant strategy and their unique magnetic performance as a function of particle size and reaction time were reported.


2013 ◽  
Vol 781-784 ◽  
pp. 280-282
Author(s):  
Zong Cheng Miao ◽  
Yi Wei Wang ◽  
Yuan Yuan Li ◽  
Lei Zhang ◽  
Xin Zhang ◽  
...  

In order to obtain the important liquid crystal intermediate with trifluoromethyl substitutent, Sonogashira coupling reaction was used to synthesize the compound. In this paper, the intermediate was synthesized by 4'-Iodo-4-pentyl-biphenyl and trimethyl silyl acetylene (TMSA) as raw materials. During the synthesis, the optimum reaction conditions were obtained, that the mol ratio of 4'-Iodo-4-pentyl-biphenyl and trimethyl silyl acetylene is 1:2, the reaction temperature is 30 oC, and the reaction time is 10 h.


2012 ◽  
Vol 550-553 ◽  
pp. 400-403 ◽  
Author(s):  
Xue Nan Sun ◽  
Li Cui ◽  
Tong Kuan Xu ◽  
Da Zhi Wang

Benzaldehyde 1, 2-propanediol acetal was synthesized from benzaldehyde and 1, 2-propanediol in the presence of ionic liquid [HMIM]HSO4. The effect of the amount of catalyst, reaction time, reaction temperature, and the molar ratio of raw materials agent on the product yield was investigated respectively. Experimental results demonstrate that ionic liquid [HMIM]HSO4is a good catalyst for preparation of benzaldehyde 1, 2-propanediol acetal. Results showed the optimal reaction conditions are as follows: the mole ratio of benzaldehyde to 1, 2-propanediol is 1:1.3, the amount of catalyst is 3.0g, the reaction temperature is 343K, and the reaction time is 4h. The achieved yield of acetal is 78. 7%.


2018 ◽  
Vol 7 (4) ◽  
pp. 316-322 ◽  
Author(s):  
Ágnes Magyar ◽  
Zoltán Hell

Abstract A series of pentasubstituted 4H-pyrans and tetrahydrobenzo[b]pyrans are synthesized with excellent yields via a one-pot condensation of aromatic aldehydes, malononitrile, and a dicarbonyl compound, ethyl acetoacetate, acetyl-acetone or dimedone, in the presence of 4 Å molecular sieve modified with zinc(II) as heterogeneous catalyst, in ethanol. The process offers numerous advantages, such as better yield, short reaction time, and mild reaction conditions. The catalyst’s preparation is simple and it could be reused while still maintaining its activity.


2013 ◽  
Vol 781-784 ◽  
pp. 283-286
Author(s):  
Xiang Wen Kong ◽  
Han Wang ◽  
Zhao Jing Li ◽  
Jing Zhang

Cyclohexyl ferulate was prepared by direct sterification of ferulic acid and cyclohexanol as raw materials with sodium bisulfate supported by silica as a catalyst. The influences of some factors on the synthesis process were studied. The optimal reaction conditions based upon 0. 2 mol of ferulic acid were chosen that the molar ratio of cyclohexanol and ferulic acid was 10 : 1, the mass ratio of catalyst to reactants was 5%, refluing reaction time was 3.5 hours, et a1. The yield of the product reached 80%. The structure of the product was characterized by IR, 1H NMR and MS spectrum. The catalyst could be recycled and used for many times, which is friendly to the environment.


2002 ◽  
Vol 2002 (2) ◽  
pp. 66-68 ◽  
Author(s):  
Nikolai Kuhnert ◽  
Timothy N. Danks

The synthesis of cyclopentadienyl bis-phosphine ruthenium thiolato complexes of the type [RuCp(dppm)SR] from [RuCp(PPh3)2 Cl] using conventional heating and microwave irradiation using a focused monomode reactor is described and the protocols compared. A considerable decrease of the reaction time is observed under microwave conditions. Yields by both methods are comparable. Functionalities such as esters, carboxylic acids and amides on the thiolato ligands are tolerated under the reaction conditions.


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