HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 86698309, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 136378639 | HCID 136378639 | — |
| Product | HCID 86698309 | HCID 86698309 | 93% |
Reaction Steps
A mixture of 2-((dimethylamino)methyl)-6,7-dimethoxyquinazolin-4-(3H)-one (100 mg) and phosphorous oxychloride (10 mL) was refluxed for 2 h. Excess of POCl3 was evaporated under vacuum and the reaction mixture was attained to rt. The mixture was poured into ice cold water and basified with aqueous ammonia solution. 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 an off-white color solid (100 mg, 93%), mp 78-80° C. 1H NMR (400 MHz, CDCl3): δ 7.41 (1H, s), 7.38 (1H, s), 4.05 (6H, s), 3.82 (2H, s), 2.42 (6H, s); LC-MS (positive ion mode): m/z 282, 284 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815879B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-c8599f16ecb8485b946e7c0f1555d530 |
| Source note | uspto-grants-2014_08 |