Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chlorodifluoromethane | HCID 6372 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 735531 | HCID 735531 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59426447 | HCID 59426447 | 40% |
Reaction Steps
Freon-22 (HCF2Cl) gas is bubbled into a solution of ethyl 5-hydroxy-1-(4-methoxyphenyl)-2-methyl-1H-indole-3-carboxylate (250 mg, 0.77 mmol) in CH2Cl2 (5 mL) at 0° C. containing a small amount of tetrabutylammonium bromide as a phase transfer catalyst. A 50% solution of NaOH is added dropwise at 0° C. After the addition, the mixture is stirred at 0° C. for 2 h. After the addition of H2O, the organic phase is separated and washed with brine and dried over Na2SO4. The solvent is then concentrated and the residue is purified by column chromatography over silica gel using EtOAc/petroleum ether (1/2) as eluent to yield the desired product in 40% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07973069B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-fbbd72d14db542fa88ce322a44ecba43 |
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| Source note | uspto-grants-2011_07 |
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