HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21412653, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 21412650 | HCID 21412650 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 21412653 | HCID 21412653 | — |
Reaction Steps
A solution of ethyl 2-(2',4'-difluoro-2-hydroxy-4-biphenylyl)propionate (2.0 g.), from the previous Example, in dry ether (40 ml.) was added over 15 minutes in dry ether (40 ml.). After stirring under reflux for 1.5 hours, excess lithium aluminium hydride was decomposed by the cautious addition of water and finally with 2N sulphuric acid (10 ml.). The product was isolated in ether, washed, dried, evaporated and distilled to give a thick translucent oil, setting to a hard glass on cooling. Trituration with boiling light petroleum (b.p. 62°-68° C.) gave a crystalline solid. This was recrystallised from methylene chloride/light petroleum (b.p. 40°-60° C.) to give 2-(2',4'-difluoro-2-hydroxy-4-biphenylyl)propan-1-ol, m.p. 118°-118.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04048332 |
| Source dataset | uspto-grants-1977_09 |
| ORD ID | ord-01251b69d97d423e9a44348995db9401 |
| Source note | uspto-grants-1977_09 |