Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 19369807 | HCID 19369807 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19369820 | HCID 19369820 | 96.8% |
Reaction Steps
1-(2-Methyl-4-hydroxyphenyl)-4-oxo-6-trifluoromethoxy-2,3,4,5-tetra-hydropyrrolo[3,2-c]quinoline(2.3g, 6.1 mmol) was dissolved in dichloromethane. Triethylamine(2.6 ml, 18.0 mmol) was added and methanesulfonyl chloride(1.0 ml, 12.8 mmol) were added, and then the reaction mixture was stirred at -78° C. for 3 hours. The reaction mixture was slowly warmed up to -10° C., and stirred for 1 hours. After extracting the reaction mixture with dichloromethane, the organic layer was washed with water for 3 times. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was crystallized in dichloromethane/hexane to obtain 2.3 g of desired compound as solid in 72% 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-e824279267f541118c05e6b3cea34172 |
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| Source note | uspto-grants-2000_01 |
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