Potassium Carbonate → HCID 16123291、化合物

反応式

[C:1]1([CH:7]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:8]2[CH2:11][CH:10]([N:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)[CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])([O-])=O.[K+].[K+].[C:30](Cl)(=[O:33])[CH2:31][CH3:32]>C(#N)C>[C:18]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[N:8]2[CH2:9][CH:10]([N:12]3[CH2:17][CH2:16][N:15]([C:30](=[O:33])[CH2:31][CH3:32])[CH2:14][CH2:13]3)[CH2:11]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

実験手順

A mixture of 1-[1-(diphenylmethyl)azetidin-3-yl]piperazine (250 mg, 0.81 mmol), K2CO3 (146 mg, 1.1 mmol), propionyl chloride (98 mg, 1.1 mmol) and acetonitrile (6 mL) was stirred at RT for 16 h. The mixture was filtered through a phase separator column and the solvent was removed by evaporation. The residue was dissolved in methylene chloride and the solution washed with aqueous NaHCO3. The organic phase was separated by using a phase separator column and then the solvent was removed by evaporation. There was obtained 216 mg (73%) of 1-[1-(diphenylmethyl)azetidin-3-yl]-4-propionylpiperazine as an oil. 1H NMR (500 MHz, CDCl3): 1.1-1.2 (t, 3H), 2.2-2.4 (m, 6H), 2.9 (t, 2H), 3.0 (m, 1H), 3.4-3.5 (m, 4H), 3.6 (b, 2H), 4.4 (s, 1H), 7.2 (m, 2H), 7.3 (m, 4H), 7.4 (m, 4H); LCMS: m/z 364 (M+1)+.