HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pivaloyl chloride → N-(4-nitro-3-(trifluoromethyl)phenyl)pivalamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pivaloyl chloride | HCID 62493 | — |
| Reactant | 4-Nitro-3-(trifluoromethyl)aniline | HCID 94955 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(4-nitro-3-(trifluoromethyl)phenyl)pivalamide | HCID 9831118 | 116.5% |
Reaction Steps
To a solution of 4-nitro-3-(trifluoromethyl)aniline (1.0 g, 4.85 mmol) in CH2Cl2 (15 mL) and TEA (2.95 g, 4.1 mL, 29.11 mmol) in a round-bottom flask at 0° C. was added trimethylacetyl chloride (1.75 g, 1.8 mL, 14.55 mmol) dropwise. The reaction mixture was warmed to room temperature and was quenched by pouring into water. The layers were separated, and the aqueous layer was extracted with DCM. The combined organic layer was dried over sodium sulfate, filtered and concentrated. The residue was then purified by silica gel column chromatography using (0-100% EtOAc/Hex.) to obtain N-(4-nitro-3-(trifluoromethyl)phenyl)pivalamide (1.64 g, 81%). LC/MS: m/z 291.1 (M+H)+ at 1.83 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08802700B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-f49686ad0d9d446ab25701c32ba1e883 |
| Source note | uspto-grants-2014_08 |