HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4-Dichlorobenzoyl chloride → HCID 45258955, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| Reactant | 2-Amino-3-Nitrophenol | HCID 4115495 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 45258955 | HCID 45258955 | 98.7% |
Reaction Steps
To a 500 mL, round-bottomed, one-necked flask equipped with a magnetic stir bar and a septum was added 2-amino-3-nitrophenol (4.25 g, 27.6 mmol), anhydrous CH2Cl2 (140 mL), 4-(dimethylamino)pyridine (3.37 g, 27.6 mmol) and 2,4-dichlorobenzoyl chloride (5.78 g, 3.87 mL, 27.6 mmol). The reaction mixture was allowed to stir at room temperature overnight. TLC analysis indicated the complete consumption of starting material. The reaction mixture was diluted with CH2Cl2 (300 mL) and the mixture was washed with H2O (2×200 mL), dried (Na2SO4), and concentrated to give 8.91 g (98.7%) of a yellow-orange solid. 1H NMR analysis indicated the material, I-113 was pure enough to carry on to the next step. 1H NMR (500 MHz, CDCl3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07598397B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-397725855d914389b4a5f2125db34ddf |
| Source note | uspto-grants-2009_10 |