63675-87-6Relevant articles and documents
Method for synthesizing D-Diphenyl formyl-tartaric acid and co-producing methyl benzoate
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Paragraph 0040-0044; 0051-0054; 0060-0065; 0075, (2019/03/23)
The invention provides a method for synthesizing D-dibenzoyl tartaric acid and co-producing methyl benzoate. The method comprises the following steps that S1 an organic solvent, D-tartaric acid and lewis acid are added into a reaction bottle, stirred and heated, benzoyl chloride is added dropwise, heat preservation is conducted for 30-90 minutes, a product is cooled to be at 0-5 DEG C, suction filtration is conducted, and a filter cake A and filtrate A are obtained; S2 methyl alcohol is added into the filter cake A and stirred for 30 minutes, suction filtration is conducted, and a filter cakeB and filtrate B are obtained; S3 the filter cake B is added into pure water, heating and back flowing are conducted for 1.5-2.5 hours, a product is cooled to be at 25-30 DEG C, suction filtration isconducted, the filter cake is dried, and D-dibenzoyl tartaric acid is obtained; and S4 an esterification reaction catalyst is added into the filtrate B, back flowing is conducted, alkali is added to adjust the pH value, atmospheric distillation is conducted, water is added to wash the product, vacuum rectification is conducted, and the methyl benzoate is obtained. The method has the advantages that the technology is simple, the operation is convenient, the condition is moderate, the product chromaticity is good, the method is environmentally friendly, the cost is low, the product yield is high, and the product purity is high.
Direct synthesis of 3-acylbenzothiophenes: Via the radical cyclization of 2-alkynylthioanisoles with α-oxocarboxylic acids
Liu, Wei,Hu, Yao-Qian,Hong, Xiao-Yi,Li, Guo-Xing,Huang, Xiao-Bo,Gao, Wen-Xia,Liu, Miao-Chang,Xia, Yuanzhi,Zhou, Yun-Bing,Wu, Hua-Yue
supporting information, p. 14148 - 14151 (2019/01/03)
A radical cascade cyclization of 2-alkynylthioanisoles with α-oxocarboxylic acids with AgNO3 has been described. This reaction provides a novel route to directly access 3-acylbenzothiophenes from simple chemical feedstocks. In particular, the utility of the approach was demonstrated by its application to the synthesis of a polymerization inhibitor and a raloxifene precursor.
An air-tolerant approach to the carbonylative suzuki-miyaura coupling: Applications in isotope labeling
Ahlburg, Andreas,Lindhardt, Anders T.,Taaning, Rolf. H.,Modvig, Amalie E.,Skrydstrup, Troels
, p. 10310 - 10318 (2013/11/06)
Carbonylative Suzuki-Miyaura coupling conditions have been developed that proceed without the exclusion of oxygen and in the presence of nondegassed and nondried solvents. By adapting the method to a two-chamber setup, the direct handling of carbon monoxide, produced from stable CO precursors, is avoided. The protocol afforded the desired benzophenones with excellent functional group tolerance and in good yields. Substituting the CO precursor, in the CO-producing chamber, with its carbon-13 labeled version generated the corresponding carbon-13 labeled benzophenones. Finally, the developed system was applied in the synthesis and isotope labeling of two pharmaceuticals, nordazepam and Tricor.
