HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 59857990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178486376 | HCID 178486376 | — |
| Product | HCID 59857990 | HCID 59857990 | 84% |
Reaction Steps
A mixture of 7-bromo-8-methoxy-2-quinolinol (4c) (2.22 g, 8.7 mmol) and POCl3 (7 mL) was heated under reflux for 1.5 hours. After neutralization with NaHCO3 and extraction with AcOEt, the residue was dissolved in CHCl3 and filtered through silica gel to remove the brown polar impurities. The product (1.99 g, 84% yield) was obtained as white crystals upon recrystallization from AcOEt-Hexanes. mp 130-132° C.; 1H NMR (400 MHz, CDCl3), 8.06 (d, J=8.8 Hz, 1H), 7.66 (d, J=9.2 Hz, 1H), 7.42 (d, J=9.2 Hz, 1H), 7.39 (d, J=8.8 Hz, 1H), 4.17 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183379B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-a20d58d257d14a48a5dd737ccd9d59c8 |
| Source note | uspto-grants-2012_05 |