HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 67076299, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | [3-(2-Hydroxy-2-methylpropyl)phenyl]acetic acid | HCID 46938719 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67076299 | HCID 67076299 | 39.8% |
Reaction Steps
The compound of step 1 (0.132 g, 0.634 mmol) was dissolved in THF (0.5 ml) and added to a refluxing suspension of lithium aluminium hydride (122 mg, 3.1 mmol) in THF (1 ml). The mixture was stirred for 1 h under reflux and cooled to room temperature. Diethyl ether (6 ml) was added, followed by EA (0.4 ml). Subsequently, water was added slowly until the alumina salts formed a thick slurry from which the supernatant could be decanted easily. The slurry was repeatedly washed with EA, the combined extracts were dried with sodium sulfate and evaporated to dryness. The residue was purified by RP HPLC (water/ACN gradient) to yield 49 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362073B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-ce89ab0eebd249e89dd3e0b509ecedf1 |
| Source note | uspto-grants-2013_01 |