Sodium Methoxide → 8-(2,5-Dimethyl-phenyl)-3-methoxy-tetrahydro-pyrazolo[1,2-a][1,2,5]triazepine-7,9-dione
反応式
C(O[C:4]([N:6]1[CH2:12][CH2:11][N:10]([O:13][CH3:14])[CH2:9][CH2:8][N:7]1[C:15](=[O:25])[CH2:16][C:17]1[CH:22]=[C:21]([CH3:23])[CH:20]=[CH:19][C:18]=1[CH3:24])=[O:5])C.C[O-].[Na+]>CN(C)C=O>[CH3:24][C:18]1[CH:19]=[CH:20][C:21]([CH3:23])=[CH:22][C:17]=1[CH:16]1[C:4](=[O:5])[N:6]2[CH2:12][CH2:11][N:10]([O:13][CH3:14])[CH2:9][CH2:8][N:7]2[C:15]1=[O:25]参加物
4
実験手順
To a solution of 2-[2-(2,5-dimethyl-phenyl)-acetyl]-5-methoxy-[1,2,5]triazepane-1-carboxylic acid ethyl ester (800 mg, 2.29 mmol) in absolute dimethylformamide (10 ml) at 10° C. was added sodium methoxide (371 mg, 6.87 mmol) in one portion and stirring continued at 10° C. for 30 minutes, then at room temperature for two hours. The solvent was evaporated in vacuo, the residue diluted in cold water (10 ml), acidified to pH 5 with 2N HCl and thoroughly extracted with ethyl acetate. The combined organic layers were washed with brine (3×15 ml), dried over sodium sulfate and concentrated. The residue was triturated with diethyl ether, filtered, washed with cold ether and dried in vacuo. Yield: 450 mg of 8-(2,5-dimethyl-phenyl)-3-methoxy-tetrahydro-pyrazolo[1,2-a][1,2,5]triazepine-7,9-dione (title compound P2.4) as an off-white solid, mp 167-169° C.