HRID1598947

反应详情

EQUATION

反应方程式

HRID 1598947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.4 g (0.1 mol) of cyanoguanidine and 35.5 g (0.25 mol) of ethyl trifluoroacetate are initially introduced into 46 g of ethanol, and a suspension of 8.5 g (0.125 mol) of sodium ethoxide in 39.8 g of ethanol is added in the course of 5 min. After the addition of 5.66 g (0.05 mol) of calcium chloride, the reaction mixture is heated to reflux for 7 hours. 0.5 ml of a conc. hydrochloric acid is then added at 20° C. and the ethanol is removed. 100 g of water are added and the suspension is filtered with suction. The residue is washed with 50 ml of water and dried at 50° C./20 mbar. 18.6 g (0.089 mol, 89%) of 2-amino-4-ethoxy-6-trifluoromethyl-1,3,5-triazine are obtained in the form of a colorless powder (HPLC: 99.8 area %, m.p. 124°-125° C.).

WORKUP

后处理

  1. additionis added in the course of 5 min
  2. temperaturethe reaction mixture is heated
  3. temperatureto reflux for 7 hours
  4. customthe ethanol is removed
  5. addition100 g of water are added
  6. filtrationthe suspension is filtered with suction
  7. washThe residue is washed with 50 ml of water
  8. customdried at 50° C./20 mbar