HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → 2-Methyl-4-(1-methylcyclopropyl)benzoyl chloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | 2-Methyl-4-(1-methyl-cyclopropyl)-benzoic acid | HCID 59216436 | — |
| Product | 2-Methyl-4-(1-methylcyclopropyl)benzoyl chloride | HCID 59216504 | 81.8% |
Reaction Steps
2-Methyl-4-(1-methyl-cyclopropyl)-benzoic acid (2.139 g, 11.243 mmol) and phosphoruspentachloride (2.575 g, 12.37 mmol) were charged into a 50 ml flask under stirring. These both solids dissolved at 100° C. The reaction mixture was stirred 2 hours at 120° C. with an reflux condenser in a N2 atmosphere. After that the resulting phosphorus oxylchloride was distilled off at 140° C. from the reaction mixture. The whole reaction mixture was cooled to room temperature and the reaction mixture still remained as a solution. The desired product was distilled by Kugelrohr distillation (150° C./4 mbar) to give 2-Methyl-4-(1-methyl-cyclopropyl)-benzoyl chloride (1.92 g, 9.2 mmol)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08536166B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-386005508ce64928b3352b53594387be |
| Source note | uspto-grants-2013_09 |