化工社化工社 化学情報印刷レポート · 研究参考用
Toluene → Benzeneacetonitrile, 2,3-dichloro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Guanidine Hydrochloride | HCID 5742 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-(2,3-Dichlorophenyl)-3-ethoxy-4-fluoro-2-butenenitrile | HCID 54395328 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Benzeneacetonitrile, 2,3-dichloro- | HCID 229020 | 38% |
反応手順
To guanidine hydrochloride (25.4 kg, 266 mole) in methanol (60 litres) was added 30% w/w sodium methoxide in methanol solution (49.2 kg, 273.3 mole). The suspension was heated to 55° C.±2° C. The toluene solution of 2-(2,3-dichlorophenyl)-3-ethoxy-4-fluoro-2-butenenitrile was added over a period of 45 minutes and the resultant mixture was boiled under reflux for 4 hours, cooled then quenched into water (230 litres). The solid precipitate was washed with 5 portions of methanol (25 litres) to yield the racemate as an off white solid (26.3 kg, 38% yield from 2,3-dichlorophenylacetonitrile).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093268B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-59ccc84137fc44f3bbafa9eb91f1ac1a |
| 出典メモ | uspto-grants-2012_01 |