Potassium Carbonate → HCID 9841532、化合物

反応式

[CH2:1]([N:3]([CH2:32][CH3:33])[C:4]([C:6]1[CH:7]=[N:8][C:9]([C:12]2([C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([OH:31])[CH:26]=3)[CH2:17][CH2:16][N:15](CC3C=CC=CC=3)[CH2:14][CH2:13]2)=[N:10][CH:11]=1)=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].ClC(OC(Cl)C)=O>ClCCCl>[CH2:32]([N:3]([CH2:1][CH3:2])[C:4]([C:6]1[CH:7]=[N:8][C:9]([C:12]2([C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([OH:31])[CH:26]=3)[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]2)=[N:10][CH:11]=1)=[O:5])[CH3:33]

参加物

実験手順

To a stirring solution of 2-[1-Benzyl-4-(3-hydroxy-phenyl)-piperidin-4-yl]-pyrimidine-5-carboxylic acid diethylamide (105 mg, 0.24 mmol) in 5 mL 1,2-dichloroethane at room temperature was added potassium carbonate (K2CO3) (331 mg, 2.4 mmol) and 1-chloroethyl chloroformate (0.16 mL, 1.44 mmol). The mixture was refluxed for 24 hours, cooled to room temperature, filtered and concentrated. The resulting residue was taken up in 15 mL MeOH and refluxed for 24 hours. The mixture was cooled to room temperature and concentrated under reduced pressure to yield 86 mg (91%) of the desired amine. 1HNMR (400 MHz, CD3OD) δ 8.78 (s, 2H), 7.04 (t, 1H), 6.82-4.79 (comp, 2H), 6.54 (d, 1H), 3.55-3.32 (comp, 2H), 3.33-3.29 (comp, 2H), 2.99-2.93 (comp, 4H), 2.68 (t, 2H), 2.21 (t, 2H), 1.24-1.15 (comp, 6H); MS (M+1) 355.3