HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67542123, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Proton sponge | HCID 88675 | — |
| Reactant | Benzenepropanol, 2-(hydroxymethyl)- (9CI) | HCID 10419543 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67542123 | HCID 67542123 | — |
Reaction Steps
To a suspension of the title A compound, 3-(2-hydroxymethyl-phenyl)-propan-1-ol (14.9 g, 90 mmol) and proton-sponge (25 g, 1.3 eq.) in methylene chloride (500 mL) is added at 0° C. under nitrogen trimethyloxonium-tetrafluoroborate (17.3 g, 117 mmol). The reaction mixture is further stirred for 5 h at room temperature before filtration. The filtrate is poured into water and the aqueous layer extracted twice with methylene chloride. The combined organic extracts are dried over Na2SO4, filtered and concentrated under reduced pressure. The residue is purified by flash column chromatography on silica gel (hexane/EtOAc 7/3 to 1/1 and to AcOEt/MeOH 9/1) to afford the title compound: TLC, Rf (hexane/AcOEt 4/1)=0.57. MS 198.0 [M+18].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362040B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-5eec32501cac4ca1bede7057d759022a |
| Source note | uspto-grants-2013_01 |