反应详情

Methanesulphonyl cloride (0.28 ml) was added dropwise to a solution of 7-amino-3-(5-aminobenzofur-2-ylmethyl)-1,2,4,5-tetrahydro-3H-3-benzazepine (0.56 g) in pyridine (40 ml) cooled to 0° and the mixture was then stirred at room temperature for 18 hours. The solvent was evaporated in vacuo and the residue taken up in methylene chloride, washed three times with aqueous sodium bicarbonate and three times with brine. The organic layer was dried (Na2SO4), filtered and evaporated in vacuo to give an oil which was purified by column chromatography on silica eluting with methylene chloride containing methanol (0% up to 4%). The product-containing fractions were combined and evaporated to give the title compound as a foam, yield 0.56 g.

1. temperaturecooled to 0°
2. customThe solvent was evaporated in vacuo
3. washwashed three times with aqueous sodium bicarbonate and three times with brine
4. dry with materialThe organic layer was dried (Na2SO4)
5. filtrationfiltered
6. customevaporated in vacuo
7. customto give an oil which
8. customwas purified by column chromatography on silica eluting with methylene chloride
9. additioncontaining methanol (0% up to 4%)
10. customevaporated