反应详情

To the reaction mixture of Example 10 was added 2-n-butyl-4-chloro-1H-imidazole-5-carboxaldehyde (0.01 m=1.86 g). The reaction was stirred overnight at room temperature. Water (0.87 mL) was added dropwise followed by sodium borohydride pellets (0.37 g). After stirring for 5 hours, the reaction mixture was added slowly to 100 mL water containing 3 mL acetone. The temperature was maintained at about 25° C. during the addition. The resultant slurry was stirred for an additional 45 minutes, then filtered. The solid was rinsed with two 50 mL portions of water. The wet cake was recrystallized first from 50 mL of n-butyl chloride, then from 30 mL of ethyl acetate to give 1.95 g title compound in 28% overall yield; mp 168°-169° C.

1. stirringAfter stirring for 5 hours
2. temperatureThe temperature was maintained at about 25° C. during the addition
3. stirringThe resultant slurry was stirred for an additional 45 minutes
4. filtrationfiltered
5. washThe solid was rinsed with two 50 mL portions of water
6. customThe wet cake was recrystallized first from 50 mL of n-butyl chloride