HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl Bromide → HCID 57269970, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl Bromide | HCID 7498 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 54416206 | HCID 54416206 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57269970 | HCID 57269970 | 83% |
Reaction Steps
A mixture of the above alcohol (621 g) and sodium hydride (141 mg, 60% dispersion in oil) and benzyl bromide (0.41 ml) in dry N,N-dimethylformamide (2.5 ml) was stirred for 10 hrs at room temperature. After the mixture was cooled to 0° C., the reaction was quenched by addition of water. The pH of the mixture was adjusted to pH 7 with 0.1N hydrochloric acid. The mixture was extracted with diethyl ether, and the combined organic layers were washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. Purification of the residue by flash column chromatography (using n-hexane:ethyl acetate=20:1 as an eluent) gave benzyl [(1S,2R,6R)-2-methoxy-3,3-dimethyl-6-(1-methylvinyl)cyclohexyl]methyl ether (726 mg, 83% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05719291 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-8f1c2b221e764dc897b6203415c44ee6 |
| Source note | uspto-grants-1998_02 |