HRID392067

反应详情

EQUATION

反应方程式

HRID 392067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of intermediate 14 (6 g) in THF (250 ml) was hydrogenated with Raney nickel (3 g) as a catalyst. After uptake of hydrogen (2 equivalents), the catalyst was filtered off and the filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent CH2Cl2/(CH3OH/NH3) 90/10). The pure fractions were collected and the solvent was evaporated, yielding 4 g (68%) [1-(2-amino-ethyl)-4-piperidinyl]methyl 8-amino-7-chloro-2,3-dihydro-1,4-benzodioxin-5-carboxylate (intermediate 15).

WORKUP

后处理

  1. customthe filtrate was evaporated
  2. customThe residue was purified by column chromatography over silica gel (eluent CH2Cl2/(CH3OH/NH3) 90/10)
  3. customThe pure fractions were collected
  4. customthe solvent was evaporated