Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 6-Fluoroindole | HCID 351278 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 44596115 | HCID 44596115 | — |
Reaction Steps
To a solution of 6-fluoroindole (1.18 g, 8.56 mmol) in dry THF (65 mL) at 0° C. under argon was added (COCl)2 (0.93 mL, 10.7 mmol). The reaction mixture was stirred at 0° C. for 2 h and at rt for 15 h. The reaction mixture was cooled to 0° C. and EtOH (0.90 mL, 15.5 mmol) was added. The reaction mixture was stirred at rt for 24 h, then poured into cold satd NaHCO3. The mixture was extracted with EtOAc. The combined EtOAc extracts were washed with satd aq NaHCO3 and brine, dried, and evaporated to give the title compound: TLC Rf=0.48 (19:1 CH2Cl2/Me2CO); MS (ESI−) m/z 234.0; 1H NMR (CDCl3, 300 MHz) δ 10.95 (1H), 8.38 (1H), 8.31 (1H), 7.07 (1H), 4.37 (2H), 1.39 (3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06586421B2 |
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| Source dataset | uspto-grants-2003_07 |
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| ORD ID | ord-00a97eeff3464ec8a9ea4817ee8df1c1 |
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| Source note | uspto-grants-2003_07 |
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