HRID2239833

反应详情

EQUATION

反应方程式

HRID 2239833 的结构方程式

PROCEDURE

实验过程

N,N-Dimethylaniline (601 mg, 4.96 mmol) was added to a suspension of 2-(methylthio)pyrazolo[1,5-a][1,3,5]triazin-4(3H)-one (1.88 g, 10.33 mmol) from 1c in POCl3 (29 mL). The reaction mixture was heated to reflux for 7 hours, and then cooled to room temperature, concentrated in vacuo, and diluted with cold water (110 mL). The resulting solid was collected by vacuum filtration, washed with cold water and hexane, and then air dried to give 1.68 g (81%) of 4-chloro-2-(methylthio)pyrazolo[1,5-a][1,3,5]triazine.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 7 hours
  3. concentrationconcentrated in vacuo
  4. additiondiluted with cold water (110 mL)
  5. filtrationThe resulting solid was collected by vacuum filtration
  6. washwashed with cold water and hexane
  7. customair dried