反应详情

90.4 mg of 2,3,5,10,11,11a-hexahydro-9-hydroxy-11-methoxy-8-methyl-1H-pyrrolo(2,1-C)(1,4)benzodiazepin-5-one was dissolved in 15 ml of acetonitrile at an elevated temperature. After dissolution, the solution was concentrated first at ordinary pressure and then under a reduced pressure. The concentrate was dissolved in 1.5 ml of hot benzene, and then 25 ml of n-hexane was added thereto, and the separated precipitate was collected by filtration. This procedure was repeated 2 to 3 times, and there was obtained 63.5 mg of 2,3,5,11a-tetrahydro-9-hydroxy-8-methyl-1H-pyrrolo(2,1-C)(1,4)benzodiazepin-5-one as a light yellow powdery product. It had a melting point of 147.5° to 150° C.

1. dissolutionAfter dissolution
2. concentrationthe solution was concentrated first at ordinary pressure
3. dissolutionThe concentrate was dissolved in 1.5 ml of hot benzene
4. addition25 ml of n-hexane was added
5. filtrationthe separated precipitate was collected by filtration