反应详情

Methanesulphonyl chloride (0.56 ml) was added dropwise to a solution of 7-amino-3-tertiary-butoxycarbonyl-1,2,4,5-tetrahydro-3H-3-benzazepine (1.9 g) in pyridine (40 ml) cooled to 0°. Stirring was continued at room temperature for 18 hours. The solvent was removed by evaporation to give an oil which was taken up in methylene chloride, washed three times with aqueous sodium bicarbonate and three times with brine, then dried (Na2SO4) and evaporated in vacuo. The residue was purified by column chromatography on silica eluting with methylene chloride containing methanol (0% up to 5%). The product-containing fractions were combined and evaporated in vacuo to give a semi-solid which was triturated with ether to give the title compound, yield 1.2 g, m.p. 153°-154°.

1. temperaturecooled to 0°
2. customThe solvent was removed by evaporation
3. customto give an oil which
4. washwashed three times with aqueous sodium bicarbonate and three times with brine
5. dry with materialdried (Na2SO4)
6. customevaporated in vacuo
7. customThe residue was purified by column chromatography on silica eluting with methylene chloride
8. additioncontaining methanol (0% up to 5%)
9. customevaporated in vacuo
10. customto give a semi-solid which
11. customwas triturated with ether