反応式
[NH2:1][C:2]1[NH:6][N:5]=[N:4][N:3]=1.[H-].[Na+].[CH3:9][O:10][C:11]1[CH:20]=[CH:19][C:14]([C:15](OC)=[O:16])=[C:13]([O:21][CH:22]([CH3:24])[CH3:23])[CH:12]=1.Cl>CS(C)=O.C(O)C>[CH3:9][O:10][C:11]1[CH:20]=[CH:19][C:14]([C:15]([NH:1][C:2]2[NH:6][N:5]=[N:4][N:3]=2)=[O:16])=[C:13]([O:21][CH:22]([CH3:24])[CH3:23])[CH:12]=1参加物
反応条件
- 温度
- 25 °C
実験手順
A solution of 3.0 g (35.3 mmol) of anhydrous 5-aminotetrazole in 20 ml of dimethyl sulfoxide is added dropwise to a 15° to 20° C. slurry of 2.8 g (70.0 mmol) of 60% NaH (oil dispersion) in 75 ml of dimethyl sulfoxide under nitrogen atmosphere. The resulting mixture is stirred at 25° C. for 2.5 hours. A solution of 6.50 g (28.98 mmol) of methyl 4-methoxy-2-(1-methylethoxy)benzoate in 25 ml of dimethyl sulfoxide is added dropwise to the reaction and stirred at 25° C. for 18 hours. The reaction is poured onto 600 g of ice-water and the resulting aqueous solution is acidified with aqueous 10% HCl. The product is isolated by vacuum filtration and recrystallization from 95% ethanol gives 1.90 g (8.03 g theoretical, 24%) of the analytically pure 4-methoxy-2-(1-methylethoxy)-N-1H-tetrazol-5-ylbenzamide as fine, white needles having a melting point of 212° -213° C.
後処理
- stirringstirred at 25° C. for 18 hours
出典と根拠
- ORDレコード
- ord-ac4c27ac2f6f4849b7ba4003c0c8aa14
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04764525
関連ノート
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