反应详情

N-(4-Methanesulphonamidophenacyl)-N-methyl-benzylamine (14.5 g) in ethanol (300 ml) containing 10% palladium on charcoal (2.0 g) was stirred under a hydrogen atmosphere (50 psi) at room temperature for 18 hours. Further catalyst (1.0 g) was added and hydrogenation was continued for a further 18 hours. The reaction was filtered and evaporated to afford an oil which was chromatographed on silica [Merck `Kieselgel 60` (Trade Mark)], eluting with methylene chloride containing methanol (0% up to 20%) to give, after collection and evaporation of appropriate fractions, the title compound as a solid, yield 5 g. [Washing the column with methylene chloride:methanol:acetic acid (80:20:0.25) gave a further 4 g of the product as the acetate salt].

1. waithydrogenation was continued for a further 18 hours
2. filtrationThe reaction was filtered
3. customevaporated
4. customto afford an oil which
5. customwas chromatographed on silica [Merck `Kieselgel 60` (Trade Mark)],
6. washeluting with methylene chloride
7. additioncontaining methanol (0% up to 20%)
8. customto give
9. customafter collection and evaporation of appropriate fractions
10. wash[Washing the column with methylene chloride:methanol:acetic acid (80:20:0.25)