HRID1892309

反应详情

EQUATION

反应方程式

HRID 1892309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

To a suspension of 6-iodo-quinoline (1.0 g, 4 mmol) and Cu(0) (559 mg, 8.8 mmol) in dry DMSO was added bromodifluoro-acetic acid ethyl ester (893 mg, 4.4 mmol). The reaction mixture was stirred under N2 at 55° C. for 15 h. The mixture was poured in a solution of K2CO3 and extracted with EtOAc. The organic layer was collected and dried over MgSO4. The crude was purified by silica gel column to give the title compound as a red oil (310 mg, 30%). 1H-NMR (400 MHz, CDCl3) δ ppm 1.33 (t, 3H), 4.334 (q, 2H), 7.52 (m, 1H), 7.93 (m, 1H), 8.15 (s, 1H), 8.20-8.23 (m, 2H), 9.03 (s, 1H).

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. customThe organic layer was collected
  3. dry with materialdried over MgSO4
  4. customThe crude was purified by silica gel column