HRID500544

反应详情

EQUATION

反应方程式

HRID 500544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

The title compound of example 23.1 (18.35 g, 109.8 mmol) and methyl isothiocyanate (8.83 g, 120 mmol) were stirred together at 60° C. for 30 minutes. Sodium hydroxide (4.83 g, 120 mmol) in water (32 mL) was added to the reaction mixture it was allowed to continue to stir at 60° C. for 12 hours. The reaction mixture was concentrated and diluted with water. It was acidified to pH 4-5 with 3 M HCl. A solid precipitated out which was filtered, washing with portions of water, then dried to afford the product as a beige solid (21.2 g, 87%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with water
  3. customA solid precipitated out which
  4. filtrationwas filtered
  5. washwashing with portions of water
  6. customdried