Acetic Anhydride → HCID 10633310、化合物
反応式
[NH2:1][C:2]1[C:7]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:6][C:5]([Cl:12])=[CH:4][N:3]=1.[C:13](OC(=O)C)(=O)[CH3:14]>>[Cl:12][C:5]1[CH:4]=[N:3][C:2]2[NH:1][C:13]([CH3:14])=[N:11][S:8](=[O:9])(=[O:10])[C:7]=2[CH:6]=1参加物
3
実験手順
A mixture of 1 g of 2-amino-5-chloropyridine-3- sulfonamide (Preparation 20) and 10 cm3 of acetic anhydride is brought to reflux for 6 hours. After cooling, the crystals are filtered off, washed with a small amount of acetic anhydride and then with diethyl ether and dried. The crystals are redissolved in 50 cm3 of 0.1N NaOH. The possible insoluble material is removed by filtration. The filtrate, adjusted to a pH of 4 using formic acid, allows crystals to precipitate. They are collected on a filter, washed with water and dried.
後処理
- temperatureto reflux for 6 hours
- temperatureAfter cooling
- filtrationthe crystals are filtered off
- washwashed with a small amount of acetic anhydride
- dry with materialwith diethyl ether and dried
- dissolutionThe crystals are redissolved in 50 cm3 of 0.1N NaOH
- customThe possible insoluble material is removed by filtration
- customto precipitate
- customThey are collected on a filter
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-c361a3ef5cf040938c8c96b9710db92f
- 出典データセット
- uspto-grants-1995_10
- 特許番号
- US05459138
反応ノート
読み込み中…