HRID639833

反应详情

EQUATION

反应方程式

HRID 639833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

3,5-difluorobenzohydrazide (5 g, 29 mol) and methyl isothiocyanate (2.1 g, 29 mmol) were mixed in 2-propanol (100 ml) and heated to 70° C. o.n. The reaction was cooled to r.t. and the formed precipitate was filtered off. H2O (100 mL) and NaHCO3 (4 g, 48 mmol) were added to the solid and the mixture was heated to 70° C. for 2 h. The reaction mixture was cooled to r.t., acidified with concentrated HCl and the title compound, 6.4 g (97%), was collected by filtration. LC-MS (M++1): 228

WORKUP

后处理

  1. temperatureThe reaction was cooled to r.t.
  2. filtrationthe formed precipitate was filtered off
  3. temperaturethe mixture was heated to 70° C. for 2 h
  4. temperatureThe reaction mixture was cooled to r.t.
  5. filtrationthe title compound, 6.4 g (97%), was collected by filtration