Methanol → HCID 58659460, 화합물

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FC(F)(F)C([NH:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][N:13]2[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]2)=[C:8]([C:19]([F:22])([F:21])[F:20])[CH:7]=1)=O.CO.C([O-])([O-])=O.[K+].[K+]>O>[F:22][C:19]([F:20])([F:21])[C:8]1[CH:7]=[C:6]([NH2:5])[CH:11]=[CH:10][C:9]=1[CH2:12][N:13]1[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]1

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실험 절차

To a solution of 2,2,2-trifluoro-N-(4-piperidin-1-ylmethyl-3-trifluoromethyl-phenyl)-acetamide (Stage 128.2; 1.427 g, 4.03 mmol) in boiling methanol (42 ml), 20 ml of a 1 N solution of K2CO3 in water are added dropwise. After 2 h stirring, the reaction mixture is cooled to rt, concentrated in vacuo and the residue re-dissolved in AcOEt and water. The aqueous layer is separated off and extracted twice with AcOEt. The organic phases are washed with water and brine, dried (Na2SO4) and concentrated to yield the title compound: MS: [M+1]+=259; 1H-NMR (DMSO-d6): 7.28 (d, 1H), 6.82 (d, 1H), 7.73 (dd, 1H), 5.40 (s, H2N), 3.32 (s, 2H), 2.27 (sb, 4H), 1.46 (m, 4H), 1.39 (m, 2H).