HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 11275144, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | Methyl 2,4-difluoro-3-methylbenzoate | HCID 44558846 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11275144 | HCID 11275144 | 126.5% |
Reaction Steps
To a solution of 2,4-difluoro-3-methyl-benzoic acid methyl ester from Step A (1.1 g, 5.5 mmol) in tetrahydrofuran (10 mL), cooled to −78° C. using a dry ice/acetone bath, was added lithium aluminum hydride, 1.0M in tetrahydrofuran (10 mL, 10 mmol), in a dropwise manner. The solution was stirred for two hours. The reaction was quenched by dropwise addition of ice-cold saturated sodium bicarbonate solution and was extracted with ethyl acetate. The organic layer was washed with water and brine and dried over magnesium sulfate. The slurry was filtered and concentrated to provide the alcohol as a colorless liquid (1.1 g, quantitative yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09056110B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-ff6f52e7ceea40c0b490744674a50473 |
| Source note | uspto-grants-2015_06 |