HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 86649061, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178497302 | HCID 178497302 | — |
| Product | HCID 86649061 | HCID 86649061 | 86% |
Reaction Steps
A mixture of methyl 2-(difluoro(4-fluorophenyl)methyl)-4-hydroxyquinazoline-7-carboxylate (1.1 g, 3.2 mmol) and phosphorus oxychloride (15 mL) was heated at reflux overnight. The mixture was concentrated under reduced pressure, and then toluene (20 mL) was added and evaporated under reduced pressure (2×). The residue in DCM was filtered through a pad of silica gel eluting with DCM. The filtrate was concentrated under reduced pressure to afford methyl 4-chloro-2-(difluoro(4-fluorophenyl)methyl)quinazoline-7-carboxylate (1 g, 86%). 1H NMR (300 MHz, DMSO-d6) δ 3.98 (s, 3H), 7.37 (t, 2H), 7.75 (t, 2H), 8.39 (d, 1H), 8.49 (s, 1H), 8.64 (d, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08349851B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-83526e5fe7a24277b51d2c27e121fdb3 |
| Source note | uspto-grants-2013_01 |