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Water → HCID 178484781、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dimethyldithiocarbamic acid | HCID 6599 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 4-Chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile | HCID 11035601 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | HCID 178484781 | HCID 178484781 | 80% |
反応手順
A mixture of 4-chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (0.7 g, 0.002 mol) and dimethyldithiocarbamic acid, sodium salt (0.57 g, 0.004 mol) in dimethyl formamide is heated at 50°-55° for 30 minutes, cooled to room temperature and poured into water. The resultant mixture is extracted with ethyl acetate. The combined extracts are washed with a saturated sodium chloride solution, dried (MgSO4) and concentrated in vacuo to give an orange oil residue. The residue is mixed with hot hexane, cooled and filtered to give an orange solid filtercake. Recrystallization of the solid from isopropanol gives the title product as a tan crystaline solid, 0.7 g (80% yield), mp 129°-131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05254559 |
| 出典データセット | uspto-grants-1993_10 |
| ORD ID | ord-c5fdfce118534de088564974051c350e |
| 出典メモ | uspto-grants-1993_10 |