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 crystallized 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. customcrystallized from glyme
8. customto yield 5.4 g, m.p. 211-213°