HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 4-Chloro-6,7-dimethoxy-2-methylquinazoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 6,7-Dimethoxy-2-methylquinazolin-4-ol | HCID 135427503 | — |
| Product | 4-Chloro-6,7-dimethoxy-2-methylquinazoline | HCID 10490150 | 92% |
Reaction Steps
A mixture of 6,7-dimethoxy-2-methylquinazolin-4(3H)-one (1.0 mg) and phosphorous oxychloride (20 mL) was refluxed for 3 h. The reaction mixture was attained to rt and poured into ice cold water and stirred for 10 min. The solution was extracted with chloroform (3×100 mL) and the combined CHCl3 layer was washed water, brine and dried over sodium sulfate. The solution was filtered and evaporated the solvent to give the product as a yellow color solid (1.0 g, 92%), mp 182-184° C. 1H NMR (400 MHz, CDCl3): δ 7.36 (1H, s), 7.30 (1H, s), 4.06 (6H, s), 2.81 (3H, s); LC-MS (positive ion mode): m/z 239, 241 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815879B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-7c2c79afe1b24e61bdf8e903313b691d |
| Source note | uspto-grants-2014_08 |