反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
0.1 g of 4-dimethylamino-pyridine and 0.94 g of dicyclohexylcarbodiimide were added to a solution of 1.1 g of (1R,3S) 2,2-dimethyl-3-[(dihydro-2-oxo-3-(2H)-thienylidene)-methyl]-cyclopropane-1-carboxylic acid in 10 ml of methylene chloride and then a solution of 1 g of (2-benzyl-5-thiazolyl)-methanol in 12 ml of methylene chloride was added to the mixture. The mixture was stirred for 17 hours at 20° C. and was filtered and the organic filtrate was washed with water, dried and evaporated to dryness under reduced pressure. The residue was taken upin 8 ml of a 7-3 cyclohexane-ethyl acetate mixture and the mixture was filtered. The filtrate was chromatographed over silica gel and was eluted with a 7-3 cyclohexane-ethyl acetate mixture to obtain 0.97 g of (2-benzyl -5-thiazolyl)-methyl (1R,3S) 2,2-dimethyl-3-[(dihydro-2-oxo-3-(2H)-thienylidene)-methyl]-cyclopropane-1-carboxylate with a specific rotation of [α]D20 =+38°±2° (c=0.5% in benzene).
WORKUP
后处理
- filtrationwas filtered
- washthe organic filtrate was washed with water
- customdried
- customevaporated to dryness under reduced pressure
- filtrationthe mixture was filtered
- customThe filtrate was chromatographed over silica gel
- washwas eluted with a 7-3 cyclohexane-ethyl acetate mixture