HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 13560178, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chlorobenzoyl chloride | HCID 69110 | — |
| Reactant | HCID 86740554 | HCID 86740554 | — |
| Product | HCID 13560178 | HCID 13560178 | 74% |
Reaction Steps
To a stirred solution of 9 g (0.033 mole) of N2 -[3-(dimethylamino)propyl]-N2 -phenyl-2,3-pyridinediamine and 3.9 g (0.038 mole) triethylamine in 75 ml of dry methylene chloride was added dropwise with stirring at 15°-20° C., 6.4 g (0.037 mole) of 2-chlorobenzoyl chloride. After stirring overnight, the reaction mixture was washed with water. The methylene chloride layer was extracted twice with dilute sodium hydroxide solution, washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was triturated in isopropyl ether to give 10 g (74%) of solid. A portion of this solid was recrystallized from isopropyl alcohol-isopropyl ether to give a cream colored solid, m.p. 90°-92° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04698430 |
| Source dataset | uspto-grants-1987_10 |
| ORD ID | ord-c401ca5e29a34357ab9d199a90f66931 |
| Source note | uspto-grants-1987_10 |