HRID1409535

反应详情

EQUATION

反应方程式

HRID 1409535 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated
  3. additionto the residue was added hexane
  4. filtrationThe precipitated crystals were collected by filtration
  5. customthe filtrate was purified by column chromatography on silica gel (solvent; hexane/ethyl acetate=9/1 to 7/3)
  6. customThe product and the crystals obtained