反应详情

To a slurry of 6.0 g. of 4,9-dihydro-9-methyl-4-phenylacetyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one in 100 ml. of dried tetrahydrofuran, cooled in an ice bath, is added 125 ml. of 1 M borane in tetrahydrofuran, dropwise over 10 minutes. The mixture is stirred at room temperature for one hour, refluxed for 6 hours and then stirred at room temperature for 16 hours. The reaction is decomposed by the addition of 50 ml. of 6 N hydrochloric acid and then 75 ml. of 5 N sodium hydroxide is added. Most of the solvent is evaporated, the residue is extracted with methylene chloride and the extract is evaporated to an oil. This oil is dissolved in hot hexane, filtered through diatomaceous earth and evaporated to an oil which crystallizes giving the desired product as colorless crystals, mp. 53°-56° C.

1. additionis added 125 ml
2. temperaturerefluxed for 6 hours
3. stirringstirred at room temperature for 16 hours
4. additionThe reaction is decomposed by the addition of 50 ml
5. customMost of the solvent is evaporated
6. extractionthe residue is extracted with methylene chloride
7. customthe extract is evaporated to an oil
8. dissolutionThis oil is dissolved in hot hexane
9. filtrationfiltered through diatomaceous earth
10. customevaporated to an oil which
11. customcrystallizes