HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → 5-(4-Fluorophenoxy)-2-thiophenecarboxaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Reactant | 5-(4-Fluorophenoxy)thiophene-2-carbonitrile | HCID 23130562 | — |
| Solvent | Water | HCID 962 | — |
| Product | 5-(4-Fluorophenoxy)-2-thiophenecarboxaldehyde | HCID 19422242 | 55% |
Reaction Steps
To a tetrahydrofuran (150 mL) solution of 5-(4-fluoro-phenoxy)-thiophene-2-carbonitrile (6.10 g, 27.8 mmol) described in Manufacturing Example 91-1-1 was added dropwise diisobutyl aluminum hydride (0.97 M n-hexane solution, 43.0 mL, 41.7 mmol) on a dry ice-ethanol bath (−78° C.) under nitrogen atmosphere, which was stirred for 2 hours at room temperature. The reaction solution was added to water, followed by extraction with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:5) to obtain the title compound (3.4 g, 55.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841327B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-85f5ef58a9f648cda80fb7b58b14fbb6 |
| Source note | uspto-grants-2014_09 |