反应详情

To a solution of 1-{2-[(3R,4S)-4-({[5-chloro-6-(hydroxymethyl)-3-pyridinyl]methyl}amino)-3-hydroxy-1-piperidinyl]ethyl}-7-(methyloxy)-1,5-naphthyridin-2(1H)-one (Example 7 above: 179.8 mg, 0.379 mmol) in DCM (2.5 ml) at 0° C. was added HCl (1M in diethyl ether) (0.417 ml, 0.417 mmol). The reaction mixture was stirred at rt for 30 min, the solvent was evaporated under vacuum and the crude was dispersed in hexane/DCM. The precipitated solid was isolated by filtration under vacuum and washed with DCM and hexane. The obtained solid was dried overnight at 40° C. under vacuum to give 1-{2-[(3R,4S)-4-({[5-chloro-6-(hydroxymethyl)-3-pyridinyl]methyl}amino)-3-hydroxy-1-piperidinyl]ethyl}-7-(methyloxy)-1,5-naphthyridin-2(1H)-one hydrochloride (143.7 mg, 0.282 mmol, 74.2% yield) as a white solid.

1. customthe solvent was evaporated under vacuum
2. additionthe crude was dispersed in hexane/DCM
3. customThe precipitated solid was isolated by filtration under vacuum
4. washwashed with DCM and hexane
5. customThe obtained solid was dried overnight at 40° C. under vacuum