反应详情

Phosgene gas is bubbled into 100 ml. of N,N-dimethylformamide at 5°-10° C. until 2.0 g. (0.02 mole) is absorbed and a crystalline suspension is formed. This suspension is added in portions to a stirred mixture of 4.5 g. (0.02 mole) of 2-(2-amino-5-thiadiazolyl)-1-methyl-5-nitroimidazole and 100 ml. of N,N-dimethylformamide at 25° C. After 30 minutes the reaction mixture is diluted with 200 ml. of diethyl ether, and the pale yellow solid is collected, washed with ether, and dried. Treatment of this material with 150 ml. of water and drying affords 5.0 g. (89%) of brilliant yellow solid melting at 230°-232° C.

1. customPhosgene gas is bubbled into 100 ml
2. customat 5°-10° C.
3. custom(0.02 mole) is absorbed
4. customa crystalline suspension is formed
5. additionThis suspension is added in portions to a stirred mixture of 4.5 g
6. customat 25° C
7. additionAfter 30 minutes the reaction mixture is diluted with 200 ml
8. customof diethyl ether, and the pale yellow solid is collected
9. washwashed with ether
10. customdried
11. dry with materialof water and drying
12. customaffords 5.0 g