Thionyl Chloride → HCID 12874108、化合物
反応式
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[S:7][CH:8]=[C:9]([CH2:12]O)[C:10]=1[Cl:11]>C(Cl)(Cl)Cl>[Cl:5][C:6]1[S:7][CH:8]=[C:9]([CH2:12][Cl:3])[C:10]=1[Cl:11]参加物
4
反応条件
- 温度
- 10 °C
実験手順
A mixtures of 357 g of thionyl chloride and 150 ml of chloroform is placed in a 1 liter flask and cooled to 10° C. At 10° to 15° C. and over a period of 35 minutes, a solution of 238 g of 2,3-dichloro-4-hydroxymethylthiophene in 350 ml of chloroform is added. After the exothermic reaction has subsided, the solution is stirred for 1 hour at 30° C., concentrated under reduced pressure and, after a small amount of triethylamine has been added, purified by distillation at 66° to 69° C./0.2 mbar. The yield is 192 g, equivalent to 70% of theory.
後処理
- customAfter the exothermic reaction
- concentrationconcentrated under reduced pressure
- additionafter a small amount of triethylamine has been added
- distillationpurified by distillation at 66° to 69° C./0.2 mbar
出典と根拠
- ORDレコード
- ord-435b179b4a3e4365b4b7809709c002a1
- 出典データセット
- uspto-grants-1981_05
- 特許番号
- US04268506
反応ノート
読み込み中…