HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methyl-3-butyn-2-ol → HCID 59354761, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methyl-3-butyn-2-ol | HCID 8258 | — |
| Reactant | Benzaldehyde, 4-(phenylmethoxy)- | HCID 78109 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59354761 | HCID 59354761 | 54.7% |
Reaction Steps
To a precooled −78° C. solution of 2-methylbut-3-yn-2-ol (4.71 g, 0.05 mol) in THF (250 mL), n-BuLi (51.2 mL, 0.08 mol) was added under an inert atmosphere, and the mixture stirred for 30 min. Then, 4-(benzyloxy)benzaldehyde (8.0 g, 0.037 mol) in THF was added and the mixture was stirred for an additional 3 h at RT, quenched with a saturated NH4Cl solution and concentrated in vacuo. The residue was acidified with HCl (1 N) and extracted with DCM (3×200 mL). The combined organic layers were washed with water, dried over Na2SO4 and concentrated in vacuo to obtain the crude product. The crude material was purified via silica gel column chromatography to afford 1-(4-(benzyloxy)phenyl)-4-methylpent-2-yne-1,4-diol (6 g, 54%) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071595B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-3eb8b755b7b741a580ef6c8aa2e9658c |
| Source note | uspto-grants-2011_12 |