化工社化工社 化学情報印刷レポート · 研究参考用
Methylamine → 2,6-Difluorophenylacetic acid methylamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 2,6-Difluorophenylacetyl chloride | HCID 2758321 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,6-Difluorophenylacetic acid methylamide | HCID 54384531 | — |
反応手順
25 ml of methylamine solution (33% in ethanol) are diluted with 90 ml of dichloromethane. While cooling, 9.52 g (50 mmol) of 2,6-difluorophenylacetyl chloride dissolved in 10 ml of dichloromethane are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10°. The reaction mixture is stirred for a further hour at 10° and then extracted three times with water. The organic phase is dried over magnesium sulphate and concentrated. The crude product is recrystallised from dichloromethane/petroleum ether and yields 8.57 g (92.6% of the theoretical yield) of 2,6-difluorophenylacetic acid methylamide of m.p. 163°-164°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05045556 |
| 出典データセット | uspto-grants-1991_09 |
| ORD ID | ord-107207ce0a8743cfbb6696ec1fda6878 |
| 出典メモ | uspto-grants-1991_09 |