HRID1436371

反应详情

EQUATION

反应方程式

HRID 1436371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzoyl isothiocyanate (4.28 mL, 31.8 mmol) was added under nitrogen to a solution of 2-amino-2-ethylbutan-1-ol (3.7315 g, 31.8 mmol), prepared in the previous step, in 100 mL of anhydrous tetrahydrofuran (exotherm on addition). After the addition, the reaction was refluxed for 2.5 h. After cooling to room temperature, 100 mL of hexane was added. The solid that formed was collected by filtration and dried under reduced pressure to give N-({[1-ethyl-1-(hydroxymethyl)propyl]amino}carbonothioyl)benzamide (7.1406 g, 80%) as a white solid. mp 161-163° C.; MS (ESI) m/z 281 [M+H]+.

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturethe reaction was refluxed for 2.5 h
  3. customThe solid that formed
  4. filtrationwas collected by filtration
  5. customdried under reduced pressure