HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pivalic acid → HCID 83450273, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pivalic acid | HCID 6417 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 5-Bromo-N1-methylbenzene-1,2-diamine | HCID 12198270 | — |
| Product | HCID 83450273 | HCID 83450273 | 37.6% |
Reaction Steps
To a stirred solution of 2,2-dimethylpropionic acid (304 mg) and 4-bromo-N2-methylbenzene-1,2-diamine (400 mg) was added POCl3 (5 ml), and the mixture was heated at reflux for 4 h. The mixture was then cooled to room temperature, and poured into ice-cold saturated NaHCO3 solution. The mixture was extracted with EtOAc, and the organic layer was washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/EtOAc) to give the title compound (200 mg) as a light orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365540B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-a5d19c4483a04eec9b6b449a4a4c7ee6 |
| Source note | uspto-grants-2016_06 |