HRID1680801
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
PROCEDURE
实验过程
23 g (0.1 mol) of 2,2-dimethyl-3-methylthio-cyclopropane-1,1-dicarboxylic acid dimethyl ester (prepared according to J. Chem. Soc., Chem. Comm. 1972 (7), 375) were dissolved in 25 ml of 1-oxo-1-methylphospholine and 2 ml of water and the solution was heated to 180° C. with 8 g of sodium bromide for 12 hours. The mixture was then cooled, poured into water, extracted by shaking with toluene and distilled. 12 g (=69% of theory) of 2,2-dimethyl-3-methylthiocyclopropane-1-carboxylic acid methyl ester of boiling point 75° C./3 mm Hg are obtained.
WORKUP
后处理
- temperatureThe mixture was then cooled
- extractionextracted
- distillationdistilled