HRID1507576

反应详情

EQUATION

反应方程式

HRID 1507576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 6-bromo-1-isopropyl-3,3-dimethylindolin-2-one (1.99 g, 7.08 mmol, 70%) in THF (20.0 ml) was added BINAP (227 mg, 354 μmol) and sodium tert-butoxide (1.74 g, 17.7 mmol), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (378 mg, 354 μmol) and benzylamine (766 mg, 782 μl, 7.08 mmol) under an argon atmosphere. The reaction mixture was heated to 70° C. for 18 hours. An aqueous solution of Na2CO3 was added to the reaction mixture at room temperature, the aqueous phase was extracted with tert-butyl methyl ether, the combined organic phases were dried over sodium sulfate, the solvent was evaporated and the residue purified by silica gel chromatography using ethyl acetate/heptane as eluent. The title compound was obtained as yellow foam (1.60 g).

WORKUP

后处理

  1. extractionthe aqueous phase was extracted with tert-butyl methyl ether
  2. dry with materialthe combined organic phases were dried over sodium sulfate
  3. customthe solvent was evaporated
  4. customthe residue purified by silica gel chromatography