HRID1409553
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
To a solution of (1-phenyl-cyclopentyl)-methanol (11.5 g, 64.34 mmol) in DCM (100 ml) was added TEA (17.5 ml, 130.68 mmol) and followed by methanesulfonyl chloride (MsCl) (8.9 g, 78.4 mmol) was added drop wise at 0° C. and the reaction mixture was stirred at RT for 16 h. After completion of the reaction, it was quenched with water and concentrated. Then the crude product was dissolved in DCM, extracted with DCM and the organic layer was washed with water, and brine and then dried over Na2SO4. The combined organic layer was concentrated to get crude methanesulfonic acid 1-phenyl-cyclopentylmethyl ester (10 g, crude) as a white solid.
WORKUP
后处理
- additionwas added drop wise at 0° C.
- customAfter completion of the reaction, it
- customwas quenched with water
- concentrationconcentrated
- dissolutionThen the crude product was dissolved in DCM
- extractionextracted with DCM
- washthe organic layer was washed with water, and brine
- dry with materialdried over Na2SO4
- concentrationThe combined organic layer was concentrated