HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Benzyl(2,2-difluoroethyl)amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | Chlorodifluoroethane (mixed isomers) | HCID 2736499 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | Benzyl(2,2-difluoroethyl)amine | HCID 50896648 | 70.1% |
Reaction Steps
An amount of 2 g (20 mmol) of 2,2-difluoro-1-chloroethane and 4.5 g (41 mmol) of benzylamine are heated in 62 g of N-methylpyrrolidone in an autoclave at an internal temperature of 120° C. for 16 hours. Subsequently, 50 g of 1N hydrochloric acid are added and the solvent is removed under vacuum. The residue is taken up in 50 ml of water and 50 ml of dichloromethane and adjusted to pH 8 with solid sodium hydrogencarbonate. The phases are subsequently separated and the aqueous phase is again extracted with 20 ml of dichloromethane. The organic phase is distilled. An amount of 2.4 g of N-benzyl-2,2-difluoroethanamine is obtained, which corresponds to a yield of 66.2%, based on 2,2-difluoro-1-chloroethane used.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450528B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-4557f4def249429b8ad9cf0919123195 |
| Source note | uspto-grants-2013_05 |