HRID876784

反应详情

EQUATION

反应方程式

HRID 876784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Bromine (2.08 g, 13 mmol) was dropwise added to a mixture of thieno[2,3-b]pyridine (J-2) (1.35 g, 10 mmol), dipotassium monohydrogen orthophosphate (940 mg, 5.4 mmol), sodium bicarbonate (840 mg 10 mmol), and magnesium sulfate (2.0 g, 16.7 mmol) in chloroform (40 mL) which has been stirred at reflux for 16 h, the resulting mixture was stirred under reflux for 24 h, then filtered and washed with DCM. The filtrate was concentrated, and purified by chromatography. MS (m/z): 214 (M+H)+.

WORKUP

后处理

  1. temperatureat reflux for 16 h
  2. stirringthe resulting mixture was stirred
  3. temperatureunder reflux for 24 h
  4. filtrationfiltered
  5. washwashed with DCM
  6. concentrationThe filtrate was concentrated
  7. custompurified by chromatography