HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 19369788, compound → HCID 19369826, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 19369788 | HCID 19369788 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 19369826 | HCID 19369826 | 162.4% |
Reaction Steps
1-(2,3-Dimethylphenyl)-4-oxo-6-trifluoromethoxy-2,3,4,5-tetrahydro-pyrrolo[3,2-c]quinoline(4.4 g, 11.8 mmol) was dissolved in phosphoryl chloride(10 ml). The reaction mixture was refluxed for 2 hours. After removing the excess phosphoryl chloride by simple distillation, the residue was poured into iced water, neutralized with aqueous solution of sodium hydroxide(1N), and stirred for 30 minutes. The resultant was extracted with dichloromethane(20 ml) for 3 times, and the organic layer was washed with water(15 ml) for 3 times, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography to obtain 4.0 g of desired compound as solid in 87% of yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06011044 |
| Source dataset | uspto-grants-2000_01 |
| ORD ID | ord-78fa2b69f43248b7a1cceb28c12f182d |
| Source note | uspto-grants-2000_01 |