HRID1951220

反应详情

EQUATION

反应方程式

HRID 1951220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (60% in oil, 0.538 g, 13.4 mmol) is added to a stirred solution of 2-(1H-pyrazol-3-yl)-isoindole-1,3-dione (2.39 g, 11.2 mmol) in dry DMF (25 ml) at room temperature. After 10 minutes tert-butyl bromoacetate (1.81 ml, 11.2 mmol) is added and the reaction is stirred for 18 hours. The reaction is quenched with water (1 ml), ethyl acetate (150 ml) is added and the organic phase is washed with water (3×100 ml) followed by brine (1×100 ml). The solvent is removed and the product is purified by chromatography on silica (gradient elution: ethyl acetate—hexane) to give the titled compound.

WORKUP

后处理

  1. customThe reaction is quenched with water (1 ml), ethyl acetate (150 ml)
  2. additionis added
  3. washthe organic phase is washed with water (3×100 ml)
  4. customThe solvent is removed
  5. customthe product is purified by chromatography on silica (gradient elution: ethyl acetate—hexane)