HRID1918870

反应详情

EQUATION

反应方程式

HRID 1918870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A 25 mL sealed vial was charged with (4-fluoro-6-{6-oxo-8-thia-5-azatricyclo[7.4.0.02,7]trideca-1(9),2(7)-dien-5-yl}-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-methyl acetate 212b (580 mg, 1.16 mmol), 136d (300 mg, 0.97 mmol), CH3COONa (160 mg, 1.94 mmol), K3PO4 (410 mg, 1.94 mmol), PdCl2(dppf) (100 mg, 0.12 mmol), CH3CN (12 mL), and H2O (1 mL). The mixture was heated at 110° C. for 2 hours. The reaction mixture was evaporated and the residue was purified by flash column eluting with 50:1 methylene chloride/methanol containing 0.5% triethylamine to give 136e as a black solid (300 mg, 52%).

WORKUP

后处理

  1. customA 25 mL sealed vial
  2. customThe reaction mixture was evaporated
  3. customthe residue was purified by flash column
  4. washeluting with 50:1 methylene chloride/methanol containing 0.5% triethylamine