Acetic Anhydride → N-[1,3-dimethyl-4-(4-methyl-1-cyclohexen-1-yl)-1H-pyrazol-5-yl]formamide
反応式
[CH3:1][N:2]1[C:6]([NH2:7])=[C:5]([C:8]2[CH2:13][CH2:12][CH:11]([CH3:14])[CH2:10][CH:9]=2)[C:4]([CH3:15])=[N:3]1.[C:16](OC(=O)C)(=[O:18])C>C(O)=O>[CH3:1][N:2]1[C:6]([NH:7][CH:16]=[O:18])=[C:5]([C:8]2[CH2:13][CH2:12][CH:11]([CH3:14])[CH2:10][CH:9]=2)[C:4]([CH3:15])=[N:3]1参加物
4
実験手順
To a suspension of 1,3-dimethyl-4-(4-methyl-1-cyclohexen-1-yl)-5-(1H)-pyrazolamine (24.5 g; 0.119 mole) in 99% formic acid (245 ml), acetic acid anhydride (64.14 g, 0.628 mole) is added at a temperature of about 20° C. Then the mixture is heated to 80°-90° C. and kept at this temperature for about 2 hours. After distillation of the solvent under vacuum, the residue is taken up with water and the pH is adjusted to about 8 with aqueous sodium carbonate. The solution is extracted with methylene chloride and the organic layer is washed with water and then dried over sodium sulfate. After distillation of the solvent, the crude product of the title is recovered and crystallized from the mixture t.butylmethyl-ether and hexane. M.p. 97°-99° C.