HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methoxybenzylamine → 2,2-difluoro-N-(4-methoxybenzyl)ethanamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methoxybenzylamine | HCID 75452 | — |
| Reactant | Chlorodifluoroethane (mixed isomers) | HCID 2736499 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2,2-difluoro-N-(4-methoxybenzyl)ethanamine | HCID 60923191 | 68% |
Reaction Steps
An amount of 23.15 g (214 mmol) of 2,2-difluoro-1-chloroethane and 10 g (71 mmol) of 4-methoxybenzylamine are heated in an autoclave at an internal temperature of 120° C. for 16 hours. Subsequently, 50 g of water are added and the aqueous phase is separated. The aqueous phase is again extracted with 2,2-difluoro-1-chloroethane and the combined organic phases are distilled as described in Example 1.1. Here also, the 4-methoxybenzylamine hydrochloride present in the aqueous phase can be converted back into free 4-methoxybenzylamine by addition of sodium hydroxide solution. After distillation, 4.93 g of 2,2-difluoro-N-(4-methoxybenzyl)ethanamine are obtained, which corresponds to a yield of 68%, based on reacted 4-methoxybenzylamine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450528B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-085a0b60b7cf43a18b57752ccae5b6c5 |
| Source note | uspto-grants-2013_05 |