HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → 2,6-Difluorophenylacetic acid methylamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 2,6-Difluorophenylacetyl chloride | HCID 2758321 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2,6-Difluorophenylacetic acid methylamide | HCID 54384531 | — |
Reaction Steps
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°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05098922 |
| Source dataset | uspto-grants-1992_03 |
| ORD ID | ord-e248cf9073c54ab0922c7b57752b4830 |
| Source note | uspto-grants-1992_03 |