HRID12398

反应详情

EQUATION

反应方程式

HRID 12398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of oxalyl chloride (490 μL, 5.6 mmol) in DCM (10 mL) at −78° C. was added DMSO (796 μL, 11.2 mmol) dropwise followed by the addition of a solution of 20b (943 mg, 5.6 mmol) in DCM (2 mL). The mixture was stirred at −78° C. for 30 min and TEA (3.6 mL, 25.5 mmol) was added. The reaction was stirred at −78° C. for 5 min, warmed to rt and stirred at rt for 30 min. The reaction was quenched with water and extracted with DCM. The organic layers were combined and washed with water, dried over magnesium sulfate to give 20c as a yellow semi-solid (880 mg).

WORKUP

后处理

  1. stirringThe reaction was stirred at −78° C. for 5 min
  2. temperaturewarmed to rt
  3. stirringstirred at rt for 30 min
  4. customThe reaction was quenched with water
  5. extractionextracted with DCM
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate