反应详情

温度

70 °C

A mixture of intermediate 10 (18 g) in HCl (25 ml) and THF (250 ml) was stirred for 30 minutes at 70° C. The reaction mixture was cooled, alkalized with aqueous ammonia and the layers were separated. The aqueous layer was extracted twice with THF. The combined organic layers were dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/(CH3OH/NH3) 90/10). The pure fractions were collected and the solvent was evaporated. The residue (10 g) was dissolved in CHCl3, washed with aqueous ammonia, dried, filtered and the solvent was evaporated. The residue was suspended in DIPE, filtered off and dried, yielding 8.5 g (65%) 4-piperidinylmethyl 4-amino-5-chloro-2-methoxybenzoate (intermediate 11).

1. temperatureThe reaction mixture was cooled
2. customthe layers were separated
3. extractionThe aqueous layer was extracted twice with THF
4. customThe combined organic layers were dried
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/(CH3OH/NH3) 90/10)
8. customThe pure fractions were collected
9. customthe solvent was evaporated
10. dissolutionThe residue (10 g) was dissolved in CHCl3
11. washwashed with aqueous ammonia
12. customdried
13. filtrationfiltered
14. customthe solvent was evaporated
15. filtrationfiltered off
16. customdried