HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 57771539, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 57771421 | HCID 57771421 | — |
| Product | HCID 57771539 | HCID 57771539 | — |
Reaction Steps
To a solution of spiro[4.5]dec-7-ene-8-carbonitrile (2.8 g) obtained in Step 2 in ethanol (30 mL) was added concentrated sulfuric acid (3 mL), followed by heating the reaction mixture under reflux while stirring for 5 days. After cooling down to room temperature and adding water, the reaction mixture was extracted with ethyl acetate twice. The organic layer was washed successively with saturated aqueous sodium bicarbonate solution and saturated brine, dried and concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:hexane (volume ratio)=1:4) to give spiro[4.5]dec-7-ene-8-carboxylic acid ethyl ester (2.8 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299296B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-b20f6c8199204f0c9c8a6a3e2e7f4749 |
| Source note | uspto-grants-2012_10 |