反应详情

7-Methanesulphonamido-1,2,4,5-tetrahydro-3H-3-benzazepine (0.21 g), 4-[2-(methanesulphonyloxy)ethyl]methanesulphonanilide (0.26 g) (see EP-A-0245997, Preparation 7) and triethylamine (0.12 ml) were heated at reflux temperature in ethanol for 24 hours. The solvent was removed in vacuo and the residue taken up in methylene chloride, washed with aqueous sodium bicarbonate, brine and then water. The organic layer was dried (Na2SO4), evaporated in vacuo and the residue purified by column chromatography on silica eluting with methylene chloride containing methanol (0% up to 5%). The product-containing fractions were combined and evaporated to give a solid which was recrystallised to give the title compound, yield 0.05 g, m.p. 190°-193°.

1. customThe solvent was removed in vacuo
2. washwashed with aqueous sodium bicarbonate, brine
3. dry with materialThe organic layer was dried (Na2SO4)
4. customevaporated in vacuo
5. customthe residue purified by column chromatography on silica eluting with methylene chloride
6. additioncontaining methanol (0% up to 5%)
7. customevaporated
8. customto give a solid which
9. customwas recrystallised