反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionis added in the course of 5 min
- temperaturethe reaction mixture is heated
- temperatureto reflux for 7 hours
- customthe ethanol is removed
- addition100 g of water are added
- filtrationthe suspension is filtered with suction
- washThe residue is washed with 50 ml of water
- customdried at 50° C./20 mbar