HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 4,6-difluoro-5-[4-(2-hydroxyethoxy)phenyl]-1H-indole-3-carbaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Bromo-4,6-difluoro-1H-indole-3-carbaldehyde | HCID 86698578 | — |
| Reactant | 2-[4-(5,5-Dimethyl-1,3,2-dioxaborinan-2-yl)phenoxy]ethanol | HCID 86698634 | — |
| Catalyst | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4,6-difluoro-5-[4-(2-hydroxyethoxy)phenyl]-1H-indole-3-carbaldehyde | HCID 86698633 | 38% |
Reaction Steps
A solution of 5-bromo-4,6-difluoro-1H-indole-3-carbaldehyde (150 mg, 0.58 mmol) and 2-[4-(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)phenoxy]ethanol (158 mg, 0.64 mmol) in toluene (5 mL) and EtOH (1.6 mL) was added to a solution of potassium carbonate (240 mg, 1.74 mmol) in water (1.2 mL) and Pd(dppf)Cl2 (24 mg, 0.029 mmol) at room temperature under N2. TLC (petroleum ether/EtOAc=1:1) showed the reaction was complete. The reaction was cooled to room temperature, and extracted with ethyl acetate (20 mL×2). The organic layers were washed with brine (10 mL), dried over sodium sulfate, concentrated in vacuo, and purified by column chromatography to give the title compound (70 mg, 38%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889730B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-53d67ec629ce4d348e80bb588c85104c |
| Source note | uspto-grants-2014_11 |