反应详情

A stirred mixture of 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one (0.294 mole), dry pyridine (2300 ml.) and phosphorus pentasulfide (72.4 g.; 0.323 mole) is reflexed under nitrogen for 30 minutes, cooled and concentrated in vacuo. A suspension of the residue in ice water is extracted with methylene chloride. The extract is dried over anhydrous potassium carbonate and concentrated. The residue thus obtained is crystallized from methylene chlorideethanol to give 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepine-2-thione.

1. temperaturecooled
2. concentrationconcentrated in vacuo
3. additionA suspension of the residue in ice water
4. extractionis extracted with methylene chloride
5. dry with materialThe extract is dried over anhydrous potassium carbonate
6. concentrationconcentrated
7. customThe residue thus obtained
8. customis crystallized from methylene chlorideethanol