反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH:9]([SH:13])[C:10](O)=[O:11].S(Cl)([Cl:16])=O>CN1CCCC1=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH:9]([SH:13])[C:10]([Cl:16])=[O:11]参加物
反応条件
- 温度
- 50 °C
実験手順
94.8 g of 2,5-dichlorophenylthioglycolic acid are added to 103.2 g of thionyl chloride. 0.24 g of N-methylpyrrolidone is added, and the mixture is heated at 50° C. for 2 hours and is then cooled down to 0° C. At this temperature the 2,5-dichlorophenylthioglycoloyl chloride formed is then added dropwise in the course of 1 hour to a suspension of 160 g of thionyl chloride and 77.2 g of anhydrous aluminum chloride. The suspension is stirred at 0°-5° C. for 1 hour and is then poured onto a mixture of 1,200 g of ice and 800 ml of water, the resulting mixture is stirred at 80° C. for 1 hour and is then filtered with suction, and the filter cake is washed until neutral and dried in vacuo at 50° C. This gives 88.4 g of 94.5% pure 4,7-dichloro-3-oxythionaphthene.
後処理
- temperatureis then cooled down to 0° C
出典と根拠
- ORDレコード
- ord-c1165a8de6c545ca9140d070992193a8
- 出典データセット
- uspto-grants-1986_10
- 特許番号
- US04617403
関連ノート
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