反应详情

A solution of 1,1-dimethylethyl {1-[(3-fluoro-7-oxo-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-4-yl)methyl]-4-piperidinyl}carbamate (13.35 g, containing about 12.5% dichloromethane) in dichloromethane (125 ml) was ice-cooled, treated with TFA (100 ml), stirred at room temperature for 1 hour and evaporated. The residue was shaken with aqueous sodium bicarbonate (excess) and 15% methanol/dichloromethane, separated and the aqueous extracted about 50 times with 15% methanol/dichloromethane. The combined organic phases were dried and evaporated and the residue chromatographed using dichloromethane/methanol/0.88 ammonia 9:1:0.1 to give the product (8.1 g).

1. temperaturecooled
2. customevaporated
3. stirringThe residue was shaken with aqueous sodium bicarbonate (excess) and 15% methanol/dichloromethane
4. customseparated
5. extractionthe aqueous extracted about 50 times with 15% methanol/dichloromethane
6. customThe combined organic phases were dried
7. customevaporated
8. customthe residue chromatographed