HRID1670367

反应详情

EQUATION

反应方程式

HRID 1670367 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.25 g of 1-methyl-3-(trifluoromethyl)pyrazol-5-one (8-4) and 10.23 g of Lawesson's reagent were suspended in 300 ml of anhydrous toluene. The suspension was heated under reflux for 6 hours. The reaction solution was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) to produce 4.87 g of 1-methyl-3-(trifluoromethyl)pyrazol-5-thione (8-5).

WORKUP

后处理

  1. temperatureThe suspension was heated
  2. temperatureunder reflux for 6 hours
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)