HRID1371958

反应详情

EQUATION

反应方程式

HRID 1371958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

Dissolve 6-Methanesulfonyl-indol-1-ol (5.0 g, 23.7 mmol) in triethyl phosphite (35 ml) and heat at 160° C. for 5 hours. Cool the solution to ambient temperature and dilute with diethyl ether. Wash the ether solution with brine and water followed by drying (sodium sulfate) and reducing to residue. Crystallize the residue from warm ethyl acetate to give the title compound as colorless cubes: mp 149–152° C. MS (ACPI): m/e 196.0 (M+1). Analysis for C9H9NO2S: Calcd: C, 55.37; H, 4.65; N, 7.17; found: C, 55.14; H, 4.71; N, 7.20.

WORKUP

后处理

  1. temperatureCool the solution to ambient temperature
  2. washWash the ether solution with brine and water
  3. dry with materialby drying (sodium sulfate)
  4. customCrystallize the residue
  5. temperaturefrom warm ethyl acetate