反应详情

温度

60 °C

[a] To a solution of 40 g of 5-o-chlorophenyl-7-ethyl-1,2-dihydro-3H-thieno[2,3-e][1,4]diazepin-2-one in 200 ml of pyridine is added 32 g of phosphorus pentasulfide, and the mixture is stirred at 60°C for 1 hour. After allowing to cool, the reaction mixture is poured into 2 liters of ice water with stirring. The precipitate formed is collected with suction filtration and washed with water. The precipitate is dissolved in chloroform, and the solution is washed with a saturated sodium bicarbonate and washed with water. The chloroform layer is dried over sodium sulfate and concentrated in vacuo. The residue is recrystallized from a mixture of ethanol and chloroform to give 31.4 g of 5-o-chlorophenyl-7-ethyl-1,2-dihydro-3H-thieno[2,3-e][1,4]diazepine-2-thione as yellowish crystals melting at 198°-199°C (decomposition).

1. temperatureto cool
2. stirringwith stirring
3. customThe precipitate formed
4. filtrationis collected with suction filtration
5. washwashed with water
6. dissolutionThe precipitate is dissolved in chloroform
7. washthe solution is washed with a saturated sodium bicarbonate
8. washwashed with water
9. dry with materialThe chloroform layer is dried over sodium sulfate
10. concentrationconcentrated in vacuo
11. customThe residue is recrystallized from a mixture of ethanol and chloroform