HRID1519748

反应详情

EQUATION

反应方程式

HRID 1519748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a suspension of 8-bromoisoquinoline (2.0 g, 9.7 mmol), Q-phos (68 mg, 0.096 mmol) and Pd(dba)2 (132 mg, 0.14 mmol) in dry THF (30 mL) was added 40 mL of (2-tert-butoxy-2-oxoethyl)zinc(II) bromide solution under N2 protection. The resulting mixture was heated at 80° C. overnight. The solvent was evaporated under vacuum and the crude residue was diluted with ethyl acetate (100 mL) and washed with water (3×50 mL). The combined organic layer was washed with brine, dried over Na2SO4 and the solvent was evaporated under vacuum to give a residue which was purified with silica gel chromatography to give tert-butyl 2-(isoquinolin-8-yl)acetate (1.85 g, 78%).

WORKUP

后处理

  1. customThe solvent was evaporated under vacuum
  2. additionthe crude residue was diluted with ethyl acetate (100 mL)
  3. washwashed with water (3×50 mL)
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over Na2SO4
  6. customthe solvent was evaporated under vacuum
  7. customto give a residue which
  8. customwas purified with silica gel chromatography