HRID452661

反应详情

EQUATION

反应方程式

HRID 452661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of methyl 3-[(1-benzylpiperidin-4-yl)amino]-4-nitrobenzoate (17.1 g, 46.3 mmol), 5% platinum carbon (5.13 g), tetrahydrofuran (115 mL) and methanol (115 mL) was stirred under a hydrogen atmosphere at room temperature overnight. The m reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=2/1) and recrystallized from diisopropyl ether/ethyl acetate to give the title compound (8.40 g, yield 53%) as pale-red crystals.

WORKUP

后处理

  1. customThe m reaction mixture
  2. filtrationwas filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=2/1)
  5. customrecrystallized from diisopropyl ether/ethyl acetate