HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 474081, compound → HCID 474087, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 474081 | HCID 474081 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 474087 | HCID 474087 | 91% |
Reaction Steps
In 30 ml of dry diethyl ether was dissolved 3.0 g (5.9 mmol) of the ester compound (130c), followed by addition of 230 mg (6 mmol) of lithium aluminum hydride under ice-cooling, and the mixture was stirred at room temperature for 15 minutes. The mixture was diluted with water, extracted with ethyl acetate, the extract was washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate), and further recrystallized from ethyl acetate-n-hexane to give 2.5 g of 2-(2-(2-benzyloxyethyl)-5-(3,5-dichlorophenylthio)-4-isopropyl-1H-imidazol-1-yl)ethanol (130d) as crystals (yield 91%). mp 129-130° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06147097 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-24b3825846e145ec9e49e117df53d2b2 |
| Source note | uspto-grants-2000_11 |