Trifluoroacetic acid → 4-(4-Phenoxyphenyl)piperidine
反応式
C([N:8]1[CH2:13][CH2:12][C:11]([C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:17][CH:16]=2)(O)[CH2:10][CH2:9]1)C1C=CC=CC=1.FC(F)(F)C(O)=O>>[O:21]([C:18]1[CH:19]=[CH:20][C:15]([CH:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[CH:16][CH:17]=1)[C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1参加物
3
実験手順
1-Benzyl-4-(4-phenoxy-phenyl)-piperidin-4-ol (3.47 g, 9.6 mmol, prepared in accordance with Example 7) was combined with trifluoroacetic acid (6 mL). The resulting mixture was irradiated at 130° C. in a mono-mode microwave oven for 15 min. The mixture was then concentrated under vacuum, and the obtained residue was triturated with diethyl ether (20 mL). After the solvent was removed under vacuum, the isolated product (6.6 g) was dissolved in methanol (350 mL). To this mixture was added 10% Pd/C was added (800 mg). The resulting suspension was reacted under H2 pressure (4 bar) for 5 hr at 75° C. After removing the catalyst by filtration, the filtrate was concentrated under vacuum. The obtained residue was triturated with diethyl ether (50 mL), and the precipitate was filtered and dried under vacuum. The desired product was obtained as a light yellow solid (3.26 g, 92% yield).
後処理
- customThe resulting mixture was irradiated at 130° C. in a mono-mode microwave oven for 15 min