Thionyl Chloride → 4-(Aminosulfonyl)-3-thiophenecarbonyl chloride
反応式
[NH2:1][S:2]([C:5]1[C:6]([C:10]([OH:12])=O)=[CH:7][S:8][CH:9]=1)(=[O:4])=[O:3].S(Cl)([Cl:15])=O>>[NH2:1][S:2]([C:5]1[C:6]([C:10]([Cl:15])=[O:12])=[CH:7][S:8][CH:9]=1)(=[O:4])=[O:3]参加物
3
実験手順
A mixture of 1 g. of 4-(aminosulfonyl)-3-thiophenecarboxylic acid in 20 ml of thionyl chloride is heated under reflux for 4 hours. The mixture is cooled to room temperature and is filtered. The filtrate is evaporated in a rotary evaporator and the residue is dissolved in 270 ml. of anhydrous ether. The solution is diluted with 200 ml. of petroleum ether and the precipitate which forms is collected to give 0.4 g. of product, m.p. 140; 262°-265° C.; mass spectrum CI m/e 226 MH+.
後処理
- additionA mixture of 1 g
- temperatureunder reflux for 4 hours
- filtrationis filtered
- customThe filtrate is evaporated in a rotary evaporator
- dissolutionthe residue is dissolved in 270 ml
- additionThe solution is diluted with 200 ml
- customof petroleum ether and the precipitate which forms is collected
- customto give 0.4 g
- custom262°-265° C.
出典と根拠
- ORDレコード
- ord-940f34b62c524172b0972cfe1d4a3083
- 出典データセット
- uspto-grants-1986_11
- 特許番号
- US04621142
反応ノート
読み込み中…