HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropyl Ether → HCID 19812269, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropyl Ether | HCID 7914 | — |
| Reactant | Malononitrile | HCID 8010 | — |
| Reactant | Propanoic acid, 2-bromo-2-methyl-, ethyl ester | HCID 11745 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 19812269 | HCID 19812269 | 100.6% |
Reaction Steps
To a solution of malononitrile (300 g) and acetic acid (54.6 g) in acetonitrile (2.1 l) was added sodium nitrite (313 g) at 60°-65° C. After being stirred at the same temperature for an hour, ethyl 2-bromo-2-methylpropanoate (797 g) was added to the mixture at 65° C. After being refluxed for five hours, the mixture was cooled to the ambient temperature and allowed to stand overnight. The resulting mixture was poured into a mixture of water (4.2 l) and diisopropyl ether (4.2 l). The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated under reduced pressure to give 2-(1-ethoxycarbonyl-1-methylethoxyimino)propanedinitrile (860 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05162520 |
| Source dataset | uspto-grants-1992_11 |
| ORD ID | ord-faf2b52053264cbca1be0574581c6cfc |
| Source note | uspto-grants-1992_11 |