HRID651385

反应详情

EQUATION

反应方程式

HRID 651385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Fluorobenzamide (5.0 g, 35.9 mmol) in benzene (100 ml) is added Lawesson's reagent (7,27 g, 18.0 mmol) and the resulting solution is heated to reflux for 1 hour. The solution is cooled to room temperature, concentrated and water (150 ml) added. The mixture is heated to reflux for 3 hours, and cooled to room temperature. The precipitate is filtered and dried under vacuum to yield 4-fluorothiobenzamide as a yellow solid (4.1 g, 71%). 1H NMR (CDCl3): δ 7.09 (t, 2H), 7.90(dd, 2H).

WORKUP

后处理

  1. temperaturethe resulting solution is heated
  2. temperatureto reflux for 1 hour
  3. concentrationconcentrated
  4. additionwater (150 ml) added
  5. temperatureThe mixture is heated
  6. temperatureto reflux for 3 hours
  7. temperaturecooled to room temperature
  8. filtrationThe precipitate is filtered
  9. customdried under vacuum