反应详情

Isothiocyanato-cyclopropane (4 g) was mixed with ammonia (37% in water, 8 mL) and methanol (32 mL) at 0° C. and then stirred for 16 hours at room temperature. The mixture was then cooled to 0° C., filtered, washed with a little water and dried. The Cyclopropyl-thiourea (2.06 mmol) and 4-(2-Bromo-acetyl)-benzoic acid (2.06 mmol) were mixed in THF (12 mL). After stirring at room temperature for 5 minutes the mixture was heated to 80° C. for 2 hours. The mixture was then cooled to room temperature and filtered. The solid was washed with a small amount of diethylether and dried. m/z=261.0 in MS ES+, which was characterized by hplc and MS and used in the next step without any further purification.

1. temperatureThe mixture was then cooled to 0° C.
2. filtrationfiltered
3. washwashed with a little water
4. customdried
5. stirringAfter stirring at room temperature for 5 minutes the mixture
6. temperaturewas heated to 80° C. for 2 hours
7. temperatureThe mixture was then cooled to room temperature
8. filtrationfiltered
9. washThe solid was washed with a small amount of diethylether
10. customdried
11. customused in the next step without any further purification