反应详情

To a suspension of 11.5 g of the hydrazide prepared in Example 1 in 100 ml of absolute ethanol was added a solution of 2.8 g of potassium hydroxide in 20 ml of water. After stirring several minutes, 4.8 g of carbon disulfide was added in one portion. The suspension was refluxed 4.5 hours then concentrated in vacuo. After water (about 100 ml) was added to the residue and the suspension stirred several minutes, the suspension was filtered and the filtrate was acidified with concentrated hydrochloric acid (red to litmus paper). The mixture was filtered and the residue was washed sequentially with 1×25 ml water, 1×10 ml 2-propanol and 1×10 ml ethyl ether. The suction-dried residue was recrystallized from methanol to give 3 g of the subject compound; m.p. 224°-227° C.

1. temperatureThe suspension was refluxed 4.5 hours
2. concentrationthen concentrated in vacuo
3. additionAfter water (about 100 ml) was added to the residue
4. stirringthe suspension stirred several minutes
5. filtrationthe suspension was filtered
6. filtrationThe mixture was filtered
7. washthe residue was washed sequentially with 1×25 ml water, 1×10 ml 2-propanol and 1×10 ml ethyl ether
8. customThe suction-dried residue was recrystallized from methanol