Ammonia → Benzo-1,2,3-thiadiazole-7-carboxylic acid amide
反応式
[NH3:1].C[O:3][C:4]([C:6]1[C:14]2[S:13][N:12]=[N:11][C:10]=2[CH:9]=[CH:8][CH:7]=1)=O>O1CCCC1>[S:13]1[C:14]2[C:6]([C:4]([NH2:1])=[O:3])=[CH:7][CH:8]=[CH:9][C:10]=2[N:11]=[N:12]1参加物
4
実験手順
In an autoclave, under pressure and at room temperature, 17 g of ammonia ispassed into a solution of 19.4 g of benzo-1,2,3-thiadiazole-7-carboxylic acid methyl ester in 70 ml of tetrahydrofuran. The solution is then heatedand maintained at 80°-90° C. for approximately 20 hours, an internal pressure of 55·105Pa max. building up. Partial concentration by evaporation is then carried out and the resulting precipitate is filtered off, washed with cold tetrahydrofuran and dried. 14.9 g of beige crystals having a melting point of 270°-272°C. are obtained.
後処理
- customat room temperature
- temperatureThe solution is then heatedand maintained at 80°-90° C. for approximately 20 hours
- concentrationPartial concentration
- customby evaporation
- filtrationthe resulting precipitate is filtered off
- washwashed with cold tetrahydrofuran
- customdried
- customare obtained
出典と根拠
- ORDレコード
- ord-bb81936b7eed4b80be88f27f04375034
- 出典データセット
- uspto-grants-1991_09
- 特許番号
- US05051436
反応ノート
読み込み中…