HRID390234

反应详情

EQUATION

反应方程式

HRID 390234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

A mixture of 3-(3-dimethoxymethyl-4-nitro-phenoxy)-phenylamine (0.14 mol), prepared as in Example 65, and diisopropyl ether (0.16 mol) in DCM (1000 mL) was cooled to 10° C., and carbonochloridic acid phenylmethyl ester (also known as benzyl chloroformate) (0.16 mol) was added dropwise, then the reaction mixture was stirred overnight at room temperature and washed with H2O. The organic layer was separated, dried (MgSO4), filtered off and the solvent was evaporated. The residue was purified by column chromatography (eluent: 100% CH2Cl2). The product fractions were collected and the solvent was evaporated to yield the title compound as a residue.

WORKUP

后处理

  1. additionwas added dropwise
  2. washwashed with H2O
  3. customThe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered off
  6. customthe solvent was evaporated
  7. customThe residue was purified by column chromatography (eluent: 100% CH2Cl2)
  8. customThe product fractions were collected
  9. customthe solvent was evaporated