Ammonium Chloride → HCID 66941861、化合物

反応式

C[Mg]Cl.[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)([C:17]#N)[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[NH4+].[Cl-]>C1COCC1>[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:20][CH2:21][NH:22][CH2:23][CH2:24]2)([CH3:17])[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

実験手順

15 mL methylmagnesium chloride solution (45 mmol, 3 M in THF) were added at RT to 2.37 g (7.92 mmol) 1-benzyl-4-piperazin-1-yl-piperidine-4-carbonitrile in 100 mL dry THF and the reaction mixture was stirred for 3 h. Saturated NH4Cl solution was added, the mixture was stirred for another 10 min, the aqueous phase was washed with EtOAc, combined with 4 M NaOH solution until an alkaline reaction was obtained, extracted exhaustively with DCM and the combined organic phases were dried over Na2SO4. After elimination of the desiccant and solvent the residue was further reacted without any further purification.