反应详情

A solution of racemic 1,1-dimethylethyl{(3S,4R)-1-[(3-fluoro-7-oxo-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-4-yl)methyl]-3-hydroxy-4-piperidinyl}carbamate (15.57 g) in dichloromethane (170 ml) was cooled in ice-water, treated with trifluoracetic acid (137 ml), stirred 1 hour at room temperature and evaporated to dryness. After keeping under high vacuum for 1 hour, the crude material was dissolved in methanol and run through a column of Amberlyst A21 basic resin (500 ml) (Sigma-Aldrich Co.), eluting with methanol. The solution containing the product was evaporated and the residue chromatographed on silica gel, eluting with dichloromethane/methanol/0.88 ammonia (9:1:0.1) to give product (8.96 g, 76%).

1. customevaporated to dryness
2. waitAfter keeping under high vacuum for 1 hour
3. dissolutionthe crude material was dissolved in methanol
4. washeluting with methanol
5. additionThe solution containing the product
6. customwas evaporated
7. customthe residue chromatographed on silica gel
8. washeluting with dichloromethane/methanol/0.88 ammonia (9:1:0.1)