HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69656064, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | HCID 69656486 | HCID 69656486 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69656064 | HCID 69656064 | 98% |
Reaction Steps
Under an atmosphere of nitrogen a 1M solution of DIBAL-H in toluene (10.5 ml, 10.5 mmol) was added dropwise at −70° C. over 20 min. to a stirred solution of 2-ethyl-3-(9H-fluoren-2-yl)-acrylic acid ethyl ester (1.54 g, 5.3 mmol) in dry THF (75 ml) and the mixture stirred for 45 min. Methanol (2 ml) was added, followed by 1N HCl and ethyl acetate. The aqueous phase was separated and further extracted with ethyl acetate. The combined organic phases were washed with water, dried (MgSO4), filtered and concentrated in vacuo yielding 1.3 g of 2-ethyl-3-(9H-fluoren-2-yl)-prop-2-en-1-ol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07067530B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-fb43f99e99b045dea1574fdaa2af9ef1 |
| Source note | uspto-grants-2006_06 |