HuagongsheHuagongshe Chemistry Print Report · For research reference only
Octane → 1-(2-Ethylhexyl)-3-cyano-6-methylpyrid-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Octane | HCID 356 | — |
| Reactant | 2-Methoxyethanol | HCID 8019 | — |
| Reactant | 3-Buten-2-one, 4-methoxy- | HCID 94297 | — |
| Reactant | 2-cyano-N-(2-ethylhexyl)acetamide | HCID 4590704 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(2-Ethylhexyl)-3-cyano-6-methylpyrid-2-one | HCID 20312181 | 90% |
Reaction Steps
N-(2-ethylhexyl) cyanoacetamide (60.4 g., 0.30 mole), 4-methoxy-3-butene-2-one (60.0 g., 0.60 mole), methylcellosolve (250 ml.) and 1,4-diazobicyclo [2.2.2.] octane (6.0 g.) are heated at reflux for 4 hours. Additional 4-methoxy-3-butene-2-one(30 g.) is added and reflux is continued for another 2 hours. The solvent is removed in vacuo to give an oil. The oil is dissolved in methylene chloride and extracted first with 2N-HC (150 ml.) and then with water (2 × 250 ml.). The organic layer is dried over sodium sulfate, filtered and evaporated to dryness to give a 90% yield of crude product which is characterized by nmr and ir analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04108630 |
| Source dataset | uspto-grants-1978_08 |
| ORD ID | ord-3ff1fb0d64c245e192132ff20b39bc52 |
| Source note | uspto-grants-1978_08 |