反应详情

温度

60 °C

Diphosphorus pentasulphide (32 g) is added 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 on 20 ml of pyridine, and the resulting mixture is stirred at 60° C for 1 hour, and then allowed to cool. Then, the reaction mixture is poured into 2 liters of ice water under cooling, and the precipitate is collected by suction filtration, washed well with water and dissolved in chloroform. The chloroform solution is washed with an aqueous sodium hydrogen carbonate solution and then with water, dried over sodium sulfate, and then concentrated under reduced pressure. 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 yellow crystals, melting at 198°-199° C with decomposition.

1. temperatureto cool
2. temperatureunder cooling
3. filtrationthe precipitate is collected by suction filtration
4. washwashed well with water
5. dissolutiondissolved in chloroform
6. washThe chloroform solution is washed with an aqueous sodium hydrogen carbonate solution
7. dry with materialwith water, dried over sodium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe residue is recrystallized from a mixture of ethanol and chloroform