反应详情

Water (20 mmoles) is added to a solution of 1,1,1,3-tetrachloro-3-ethoxypropane (10 mmoles) in dimethoxyethane (25 ml). The reaction mixture is stirred for 2 h under reflux. The resulting mixture is slowly added to a mixture consisting of a 4-trifluoromethylbenzamidine hydrochloride (10 mmoles), 3-trifluoromethylphenol (11 mmoles), potassium carbonate (60 mmoles) and dimethoxyethane (50 ml), which is stirred under reflux. When the addition of 3,3-dichloroacrolein solution is completed additional 4-trifluoromethylbenzamidine hydrochloride (1 mmoles) is added. The reaction mixture is stirred for 2 hours under reflux and subsequently cooled down to ambient temperature, filtered through silica, and the organic phase is concentrated in vacuo. The residue is purified by chromatography on SiO2 (petrol ethers/diisopropylether: 6/1) to yield 3,07 g (80%) of the product having a melting point of 66-67° C.

1. temperatureunder reflux
2. additionThe resulting mixture is slowly added to a mixture
3. stirringis stirred
4. temperatureunder reflux
5. additionis added
6. stirringThe reaction mixture is stirred for 2 hours
7. temperatureunder reflux
8. filtrationfiltered through silica
9. concentrationthe organic phase is concentrated in vacuo
10. customThe residue is purified by chromatography on SiO2 (petrol ethers/diisopropylether: 6/1)