HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-Chloro-4-hydroxybenzyl alchol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | Methyl 3-chloro-4-hydroxybenzoate | HCID 77580 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 3-Chloro-4-hydroxybenzyl alchol | HCID 257456 | — |
Reaction Steps
Add a solution of DIBAL-H in toluene (1.0 M, 35 mL) to a solution of methyl 3-chloro-4-hydroxybenzoate (1.9 g, 10 mmol) at 0° C. under nitrogen. Stir the reaction at 0° C. and gradually warm to ambient temperature overnight. Quench the reaction with slow addition of 0.1N aqueous HCl, add more acid to break the gel-like solid to two clear layers. Separate the organic layer, and extract the aqueous layer with EtOAc three times. Combine the organic layers, wash with brine, dry over Na2SO4, filter and concentrate to give a white solid. MS (ES−) m/z 157 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022062B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-088128e025b7472ca00d83226fadbca9 |
| Source note | uspto-grants-2011_09 |