Methanesulfonic Acid → HCID 178437843、化合物

反応式

[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]([O:9][C:10]2[CH:11]=[C:12]([CH:15]=[CH:16][CH:17]=2)[CH:13]=O)[CH2:3]1.[CH:18]1([N:23]2[C:27]([NH2:28])=[C:26]([C:29]([NH2:31])=[O:30])[C:25]([CH2:32][CH3:33])=[N:24]2)[CH2:22][CH2:21][CH2:20][CH2:19]1.CS(O)(=O)=O>C(Cl)Cl>[CH:18]1([N:23]2[C:27]3=[N:28][C:13]([C:12]4[CH:15]=[CH:16][CH:17]=[C:10]([O:9][CH:4]5[CH2:5][CH2:6][CH2:7][CH2:8][N:2]([CH3:1])[CH2:3]5)[CH:11]=4)=[N:31][C:29](=[O:30])[C:26]3=[C:25]([CH2:32][CH3:33])[NH:24]2)[CH2:19][CH2:20][CH2:21][CH2:22]1

参加物

実験手順

A mixture of 3-(1-methyl-3-hexahydroazepinyloxy) benzaldehyde (0.79 g, 3.4 mol), 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (0.5 g, 2.2 mmol), methanesulfonic acid (0.25 ml) and xylenes (25 ml) was refluxed overnight. The solvent was stripped, the residue was dissolved in CH2Cl2 and purified by column chromatography on silica gel eluting with ether, then acetone, then 0.5% Et3N/acetone to afford 0.43 g (45%) of 1-cyclopentyl-3-ethyl-6-[3-(1-methyl-3-hexahydroazepinyloxy)phenyl]pyrazolo[3,4-d]pyrimidin-4-one, m.p. 195°-196° C.