Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | HCID 19369787 | HCID 19369787 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | 220853-65-6 | HCID 10113707 | 129.2% |
Reaction Steps
1-(2-Methyl-4-methoxyphenyl)-4-oxo-6-trifluoromethoxy-2,3,4,5-tetrahydropyrrolo[3,2-c]quinoline(4.0 g, 10 mmol) was dissolved in phosphoryl chloride(10 ml). The reaction mixture was refluxed for 2 hours, and cooled. 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 at room temperature for 30 minutes. It 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 2.8 g of desired compound as solid in 70% of yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06011044 |
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| Source dataset | uspto-grants-2000_01 |
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| ORD ID | ord-809713f4e75b4b6794ac3d26d3ef99bb |
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| Source note | uspto-grants-2000_01 |
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