HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Anisoyl chloride → 4-Methoxy-N-methyl-N-(4-picolyl)benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Anisoyl chloride | HCID 7477 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N-Methylpyridine-4-methylamine | HCID 81436 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-Methoxy-N-methyl-N-(4-picolyl)benzamide | HCID 15407880 | 21.3% |
Reaction Steps
To a solution of N-methyl-N-(4-picolyl)amine (0.40 g, 3.3 mmol) and triethylamine (1.5 mL, 10.8 mmol) in CH2Cl2 (15 mL) was added 4-methoxybenzoyl chloride (1.2 g, 7.3 mmol). The resulting mixture was stirred at rt for 15 min, and then partitioned between 2.5N NaOH and Et2O. The organic extract was washed with saturated aqueous NaCl and dried (MgSO4). The solvent was removed in vacuo, and the residue was purified by flash chromatography, eluting with a solvent gradient of 2-4% MeOH/CHCl3. The material that was isolated was triturated with Et2O to provide the title compound as a light yellow solid (0.18 g, 21%): 1H NMR (CDCl3): d 8.60 (d, 2H); 7.43 (br d, 2H); 7.20 (br s, 2H); 6.90 (br d, 2H); 4.66 (br s, 2H); 3.80 (s, 3H); 3.00 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06645989B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-8cbe354afe56468b967aea18fec74870 |
| Source note | uspto-grants-2003_11 |