HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methyl-1-(4-(trifluoromethyl)phenyl)propan-2-amine → Tert-butyl 2-(2-methyl-1-(4-(trifluoromethyl)phenyl)propan-2-yl)hydrazinecarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methyl-1-(4-(trifluoromethyl)phenyl)propan-2-amine | HCID 120994 | — |
| Reactant | Tert-butyl 3-(trichloromethyl)oxaziridine-2-carboxylate | HCID 11139943 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Tert-butyl 2-(2-methyl-1-(4-(trifluoromethyl)phenyl)propan-2-yl)hydrazinecarboxylate | HCID 89808109 | — |
Reaction Steps
4.2 g of 2-methyl-1-(4-(trifluoromethyl)phenyl)propan-2-amine was dissolved in 30 mL of methylene chloride and mixed with 5.6 g (21 mmol) of separately prepared t-butyl 3-(trichloromethyl)-1,2-oxaziridine-2-carboxylate under cooling with ice. The reaction solution was stirred at room temperature for 30 minutes, washed with 10% aqueous citric acid, with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively and dried over anhydrous sodium sulfate, and methylene chloride was removed under reduced pressure. The resulting residue was purified by intermediate pressure silica gel column chromatography (silica gel 100 g, ethyl acetate:hexane) to give 1.38 g of the desired product as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09212348B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-8d4a54362d5c44198c2cc71536a3f897 |
| Source note | uspto-grants-2015_12 |