反应详情

A mixture comprising 4 g. of 4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one [U.S. Pat. No. 3,953,430 (Example 2)] in 75 ml. of tetrahydrofuran is combined with 2 g. of lithium aluminum hydride in 50 ml. of tetrahydrofuran and refluxed under nitrogen with stirring for 10 hours. A 2 ml. portion of water is carefully added dropwise with cooling followed by 2 ml. of 15% sodium hydroxide and 6 ml. of water. The mixture is filtered and the precipitate is washed thoroughly with ether. The filtrate and washings are combined, dried over sodium sulfate, filtered and concentrated to a semi-crystalline brown oil. The product is triturated with hexane producing a tan crystalline solid. This solid is recovered, washed thoroughly with hexane and dried. This crystalline material is purified by column chromatography (alumina activity II), eluting with methylene chloride:hexane (50:50). Evaporation of the solvents yields a solid which is triturated with hexane and washed with ether, giving the desired product as pale blue crystals, mp. 125°-127° C.

1. temperaturewith cooling
2. filtrationThe mixture is filtered
3. washthe precipitate is washed thoroughly with ether
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to a semi-crystalline brown oil
7. customThe product is triturated with hexane producing a tan crystalline solid
8. customThis solid is recovered
9. washwashed thoroughly with hexane
10. customdried
11. customThis crystalline material is purified by column chromatography (alumina activity II)
12. washeluting with methylene chloride:hexane (50:50)
13. customEvaporation of the solvents
14. customyields a solid which
15. customis triturated with hexane
16. washwashed with ether