反应详情

A mixture of about 3.78 g of 1H-1,2,4-triazole-1-propanamine and about 33 ml of approximately 1N sodium hydroxide in about 100 ml of methylene chloride was stirred. An about 6.9 g portion of 3,4-dichlorobenzoyl chloride was added, the mixture was stirred about 6 hours, then allowed to stand overnight. An about 10 ml portion of approximately 1N sodium hydroxide and about 100 ml of methylene chloride were added and the mixture was shaken, then allowed to separate. The organic layer was washed with two about 40 ml portions of water, dried, filtered and evaporated to a solid which was crystallized from ethyl acetate, giving about 5.0 g of the desired product as off-white crystals, mp 128°-130° C.

1. stirringthe mixture was stirred about 6 hours
2. stirringthe mixture was shaken
3. customto separate
4. washThe organic layer was washed with two about 40 ml portions of water
5. customdried
6. filtrationfiltered
7. customevaporated to a solid which
8. customwas crystallized from ethyl acetate