HRID2253303

反应详情

EQUATION

反应方程式

HRID 2253303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of tert-butyl [3-(7-amino-4,4-dimethyl-8-nitro-1,3-dioxo-3,4-dihydro-1H-isoquinolin-2-yl)propyl]-[2-(3,4-dimethoxyphenyl)ethyl]carbamate (3.60 g, 6.31 mmol) and 20% Pd(OH)2/C (0.72 g) in EtOH (100 mL) and THF (10 mL) was stirred under H2 (balloon) for 16 h. The catalyst was removed by filtration through diatomaceous earth and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography (40-63μ silica gel, hexane:EtOAc 1:1 to 1:2) to give the title compound (2.85 g, 83% yield).

WORKUP

后处理

  1. customThe catalyst was removed by filtration through diatomaceous earth
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by flash chromatography (40-63μ silica gel, hexane:EtOAc 1:1 to 1:2)