HRID390109

反应详情

EQUATION

反应方程式

HRID 390109 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Sodium hydride (60% in mineral oil, 404 mg, 10.09 mmol) was added to an ice-cold solution of EXAMPLE 33A (2.35 g, 8.41 mmol) in anhydrous DMF (20 mL) under nitrogen. The reaction mixture was stirred at 0° C. for 30 minutes and benzenesulfonyl chloride (1.19 mL, 9.25 mmol) was then added. The ice-bath was removed and the mixture was stirred at room temperature overnight. This reaction was quenched with the addition of 50 mL of water. An off white solid material was collected by filtration, washed with water and hexane, and dried to give 3.38 g of the title product. Yield: 96%. MS (DCI+) m/z 280 (M+H)+.

WORKUP

后处理

  1. customThe ice-bath was removed
  2. stirringthe mixture was stirred at room temperature overnight
  3. customThis reaction was quenched with the addition of 50 mL of water
  4. filtrationAn off white solid material was collected by filtration
  5. washwashed with water and hexane
  6. customdried