反应详情

A mixture of 10,11-dihydro-7-hydroxy-11-oxodibenzo[b,f][1,4]thiazepin (4.5g,18.5 mmoles) and lithium aluminum hydride (3.5g,92.5 mmoles) in tetrahydrofuran (200 ml) and N-ethylmorpholine (100 ml) was refluxed for 18 hours. The reaction mixture was decomposed by the addition of 12 ml of a saturated solution of ammonium chloride and 33 ml of lM sodium bicarbonate. The mixture was filtered and the salts were washed with methanol. The filtrate was evaporated to dryness and the residue was extracted several times with ether. Chromatography of the residue on silica gel, eluting with 5% methanol in chloroform, afforded the title compound, m.p. 172°-174°.

1. temperaturewas refluxed for 18 hours
2. filtrationThe mixture was filtered
3. washthe salts were washed with methanol
4. customThe filtrate was evaporated to dryness
5. extractionthe residue was extracted several times with ether
6. washChromatography of the residue on silica gel, eluting with 5% methanol in chloroform