HRID1890377

反应详情

EQUATION

反应方程式

HRID 1890377 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

3-(1H-Indol-5-yl)-azetidine-1-carboxylic acid tert-butyl ester (135 mg, 0.5 mmol) was dissolved in DMF (10 ml) and cooled to 0° C. Sodium hydride (35.7 mg, 0.74 mmol) was added, and the reaction mixture was stirred for 1 hour at 0° C. 4-Isopropyl-benzenesulfonyl chloride (98 μl, 0.55 mmol) was added slowly to the reaction mixture. Stirring was continued for 10 minutes. Cold water (100 ml) was added to the reaction mixture, and it was extracted twice with diethyl ether (80 ml). The organic layer was dried over magnesium sulphate, filtered, and the solvent was evaporated under reduced pressure to give a crystalline solid (75 mg, 33%). ESI-MS [m/z]: 355.15 [M-(Boc)+H]+.

WORKUP

后处理

  1. stirringStirring
  2. waitwas continued for 10 minutes
  3. extractionwas extracted twice with diethyl ether (80 ml)
  4. dry with materialThe organic layer was dried over magnesium sulphate
  5. filtrationfiltered
  6. customthe solvent was evaporated under reduced pressure