HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 23344098, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 3-[(2-Hydroxyethoxy)methyl]benzonitrile | HCID 28414032 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 23344098 | HCID 23344098 | — |
Reaction Steps
A solution of 3-[(2-hydroxyethoxy)methyl]benzonitrile (1 g) in MeOH (20 ml) was treated with conc. H2SO4 (10 ml) at 0° C. The solution was then allowed to warm to room temperature before heating at reflux for 10 h. Aqueous sodium carbonate was added to neutralise the cooled solution before extracting with EtOAc. The combined organic layers were then washed with water, dried (MgSO4) and concentrated in vacuo. The residue was then purified by chromatography (Biotage, 90 g) eluting with 40°C.-60° C. petroleum ether-EtOAc (3:2) to give the title compound (650 mg). LCMS RT=2.33 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07271197B2 |
| Source dataset | uspto-grants-2007_09 |
| ORD ID | ord-d181df1061e84f148cd922d7ca34c8b2 |
| Source note | uspto-grants-2007_09 |