HRID1409535
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-(tert-butoxycarbonylamino)-cyclopentanecarboxylic acid (2.29 g) in methanol (10 mL) was added dropwise 2M trimethylsilyldiazomethane solution in hexane (11.9 mL) under ice-cooling. The reaction mixture was concentrated, and to the residue was added hexane. The precipitated crystals were collected by filtration, and the filtrate was purified by column chromatography on silica gel (solvent; hexane/ethyl acetate=9/1 to 7/3). The product and the crystals obtained above were combined to give methyl 1-(tert-butoxycarbonylamino)-cyclopentane-carboxylate (2.49 g).
WORKUP
后处理
- temperaturecooling
- concentrationThe reaction mixture was concentrated
- additionto the residue was added hexane
- filtrationThe precipitated crystals were collected by filtration
- customthe filtrate was purified by column chromatography on silica gel (solvent; hexane/ethyl acetate=9/1 to 7/3)
- customThe product and the crystals obtained