反应详情

A mixture of the above 1-[2-(3,5-Dimethyl-phenyl)-1-(2,3-dimethyl-phenyl)-ethyl]-3-(2-hydroxy-ethyl)-thiourea (94.7 g) and concentrated hydrochloric acid (700 ml) was heated under reflux for 2 hours. The hydrochloric acid phase was decanted carefully and the remainder dissolved in ethyl acetate and thoroughly washed three times with potassium carbonate solution (5 wt % in water), three times with water and dried over sodium sulphate. The solvent was removed by evaporation and the remainder titurated with a solution of light petrol ether/ethyl acetate (20/1), filtrated to yield the product (4,5-dihydro-thiazol-2-yl)-[2-(3,5-dimethyl-phenyl)-1-(2,3-dimethyl-phenyl)-ethyl]-amine [specific compound example C.33 of table C] as an off-white solid (67.1 g)

1. temperaturewas heated
2. temperatureunder reflux for 2 hours
3. customThe hydrochloric acid phase was decanted carefully
4. dissolutionthe remainder dissolved in ethyl acetate
5. washthoroughly washed three times with potassium carbonate solution (5 wt % in water), three times with water
6. dry with materialdried over sodium sulphate
7. customThe solvent was removed by evaporation
8. filtrationfiltrated