Water → 4-(4-Iodo-phenyl)-4-methylaminomethyl-piperidine-1-carboxylic acid tert-butyl ester

온도

70 °C

4-(4-Iodo-phenyl)-4-{[methyl-(2,2,2-trifluoro-acetyl)-amino]-methyl}-piperidine-1-carboxylic acid tert-butyl ester (0.22 g, 0.42 mmol) was dissolved in MeOH (4.5 mL) and H2O (0.6 mL) and K2CO3 (0.29 g, 2.1 mmol, 5 eq.) was added. The mixture was stirred and heated at 70° C. for 4 h, cooled to room temperature and then partitioned between H2O (20 mL) and CH2Cl2 (20 mL). The aqueous layer was washed with CH2Cl2 (3×10 mL) and the combined organic washes were washed with saturated brine (10 mL) and dried over anhydrous Na2SO4, filtered and concentrated by rotary evaporation to give 4-(4-iodo-phenyl)-4-methylaminomethyl-piperidine-1-carboxylic acid tert-butyl ester (0.15 g, 83%). 1H NMR (CDCl3): δ 7.78 (dd, 2H), 7.18 (dd, 2H), 3.74 (m, 2H), 3.22 (m, 2H), 2.73 (s, 2H), 2.38 (s, 3H), 2.23 (m, 2H), 1.88 (m, 2H), 1.54 (s, 9H).

1. temperaturecooled to room temperature
2. custompartitioned between H2O (20 mL) and CH2Cl2 (20 mL)
3. washThe aqueous layer was washed with CH2Cl2 (3×10 mL)
4. washthe combined organic washes were washed with saturated brine (10 mL)
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated by rotary evaporation

ORD 기록

ord-c3e17fd0cc00481191818ed9d46d6cc3

출처 데이터셋

uspto-grants-2005_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06887889B2