HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → (4-((6-(Difluoromethyl)pyridin-3-yl)methoxy)-3-methoxyphenyl)methanamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Tert-butyl 4-((6-(difluoromethyl)pyridin-3-yl)methoxy)-3-methoxybenzylcarbamate | HCID 118114378 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (4-((6-(Difluoromethyl)pyridin-3-yl)methoxy)-3-methoxyphenyl)methanamine | HCID 118114096 | 83.1% |
Reaction Steps
To a stirred solution of tert-butyl 4-((6-(difluoromethyl)pyridin-3-yl)methoxy)-3-methoxybenzylcarbamate (7.32 g, 18.56 mmol) in dichloromethane (30 ml) was added trifluoroacetic acid (15 mL, 194.70 mmol). After 2 h, the reaction mixture was concentrated, and the residue was dissolved in water (75 mL). The acidic solution was extracted with diethyl ether (50 mL). The aqueous phase was retained and made basic with concentrated ammonium hydroxide solution (50 mL). The basic aqueous phase was extracted with dichloromethane (2×100 mL). The combined organic phases were dried over magnesium sulfate, filtered, and concentrated to provide 4.54 g (83%) of (4-((6-(difluoromethyl)pyridin-3-yl)methoxy)-3-methoxyphenyl)methanamine as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067914B1 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-c2ec8f68e56c4757a9143ed3a2e44cc5 |
| Source note | uspto-grants-2015_06 |