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Dimethylformamide → 3,4,5-Trichlorothiophene-2-carbonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 3,4,5-Trichloro-2-thiophenecarboxylic acid | HCID 4168584 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 3,4,5-Trichlorothiophene-2-carbonyl chloride | HCID 7010308 | — |
反応手順
A mixture of 20.4 g (0.088 mole) of 3,4,5-trichloro-2-thiophenecarboxylic acid, 7.3 mL (0.1 mole) of thionyl chloride, 0.2 mL of DMF and 80 mL of 1,2-dichloroethane was heated at reflux temperature for 3 h. The reaction mixture became a clear solution after 1 h of heating. The mixture was allowed to cool to RT, concentrated in vacuo and exposed to high vacuum to give 22.0 g (>98% wt) an oil which solidified upon standing to an off-white powder, mp 37°-41° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06329528B1 |
| 出典データセット | uspto-grants-2001_12 |
| ORD ID | ord-4b93d44677034a77880de92adf165657 |
| 出典メモ | uspto-grants-2001_12 |