反应详情

To a mixture of 9 g of 2-methyl-2-thiopseudourea sulfate in 6 ml of H2O there is added 5.7 ml of methyl chloroformate at 0° C and the mixture is stirred for 15 minutes. Then there is added 12 ml of 25% NaOH dropwise and the mixture is stirred for 15 minutes. Then there is added 6 ml of acetic acid dropwise and the mixture is stirred for 15 minutes. Then the total amount of 4-[(2,2-dichlorocyclopropyl)methyl]thio-o-phenylenediamine from above in 50 ml of methanol is added and the mixture is refluxed for 2 hours. The alcohol is removed in vacuo and H2O is added. The resulting solid is filtered off and cyystallized from glyme to yield 5.4 g, m.p. 211°-213°.

1. stirringthe mixture is stirred for 15 minutes
2. stirringthe mixture is stirred for 15 minutes
3. temperaturethe mixture is refluxed for 2 hours
4. customThe alcohol is removed in vacuo and H2O
5. additionis added
6. filtrationThe resulting solid is filtered off
7. customto yield 5.4 g, m.p. 211°-213°