反应详情

To a stirred solution of 245 mg. (0.5 mmole) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepine in 10 ml. of tetrahydrofuran containing 0.5 ml. of triethylimine at room temperature was introduced a stream of hydrogen sulfide gas until tlc indicated that all the starting material was consumed (15 minutes). Tetrahydrofuran was evaporated. The residue was partitioned between methylene chloride and water. The methylene chloride layer was dried and evaporated. Crystallization of the residue from methanol yielded, in two crops, a product having a melting point of 243°-245°.

1. customwas consumed (15 minutes)
2. customTetrahydrofuran was evaporated
3. customThe residue was partitioned between methylene chloride and water
4. dry with materialThe methylene chloride layer was dried
5. customevaporated
6. customCrystallization of the residue from methanol
7. customyielded, in two crops