HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 4-Chloro-8-iodo-7-methylquinazoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 8-Iodo-7-methylquinazolin-4(3H)-one | HCID 135742270 | — |
| Product | 4-Chloro-8-iodo-7-methylquinazoline | HCID 58466484 | 92.1% |
Reaction Steps
Phosphorous oxychloride (19.5 mL, 210 mmol) and 8-iodo-7-methylquinazolin-4(3H)-one (2.00 g, 6.99 mmol) were added to a round bottomed flask. The reaction mixture was heated at reflux for 2 h. Upon cooling, excess POCl3 was removed under reduced pressure and the remaining crude product dissolved in DCM (100 mL) and washed with ice-cold water (300 mL) to remove excess acid. The crude residue dissolved in DCM was then dried over anhydrous sodium sulfate and concentrated in vacuo to give 4-chloro-8-iodo-7-methylquinazoline (1.96 g, 92%) as an amorphous brown solid. MS (M+H)+ 305.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989461B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-5431aab719d340fea363d8eb6c42cf1c |
| Source note | uspto-grants-2011_08 |