HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aniline → 3-Methyl-N-phenylbut-2-enamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aniline | HCID 6115 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Methyl-2-butenoyl chloride | HCID 102394 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Methyl-N-phenylbut-2-enamide | HCID 12387022 | — |
Reaction Steps
To 3,3-dimethylacryloyl chloride (4.8 mL, 43.2 mmol) in dry DCM (100 mL), was added aniline (4.02 g, 43.2 mmol) followed by diisopropylethylamine (14.28 mL, 86.4 mmol). The mixture was stirred at ambient temperature for 2 hrs. Saturated sodium bicarbonate was added to quench the reaction. The organic layer was separated and washed with sat NaHCO3 (50 mL) and water (50 mL×2). The resulting solution was dried over MgSO4 and the filtrate evaporated to afford 3-methyl-but-2-enoic acid phenylamide as a brown solid in quantitative yield (7.6 g). MS: 176.0 (M+H)+; tR=2.40 min (method 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08507536B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-0f79540178d34d2cbc9ade7a67b52fab |
| Source note | uspto-grants-2013_08 |