反应详情

A 6.12 g. portion of 4,9-dihydro-4-phenylacetyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one is suspended in 100 ml. of tetrahydrofuran under argon and stirred with cooling in an ice bath. To this is added 90 ml. of 1 M diborane in tetrahydrofuran over a period of 10 minutes. The mixture is then stirred at room temperature until solution is complete, refluxed for 18 hours, cooled and 45 ml. of 6 N hydrochloric acid is added. The tetrahydrofuran is removed in vacuo and 75 ml. of 5 N sodium hydroxide is added giving the desired final product, mp. 195°-197° C.

1. temperaturewith cooling in an ice bath
2. additionTo this is added 90 ml
3. temperaturerefluxed for 18 hours
4. temperaturecooled
5. customThe tetrahydrofuran is removed in vacuo and 75 ml
6. additionof 5 N sodium hydroxide is added