HRID1809666

反应详情

EQUATION

反应方程式

HRID 1809666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

85% Hydrazine hydrate (5.1 mL, 74 mmol) was added to a solution of [3-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-3-phenyl-propyl]-carbamic acid tert-butyl ester (2.8 g, 7.4 mmol) in THF (25 mL) and MeOH (25 mL). The resulting mixture was heated at 65° C. for 6 hours. Then the precipitate was filtered, and the filtrate was concentrated under reduced pressure to give crude product which was purified by column chromatography on silica gel (dichloromethane:MeOH, 100:1, 1% NH3H2O) to give (3-amino-3-phenyl-propyl)-carbamic acid tert-butyl ester as an off-white solid. (Yield 1.7 g, 92%).

WORKUP

后处理

  1. filtrationThen the precipitate was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customto give crude product which
  4. customwas purified by column chromatography on silica gel (dichloromethane:MeOH, 100:1, 1% NH3H2O)