HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Chloride → 3-Methyl-2-(propan-2-yl)butanenitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | 2,3-Dihydro-1-methyl-1H-phosphole 1-oxide | HCID 70104 | — |
| Reactant | Ethyl 2-cyano-3-methyl-2-(propan-2-yl)butanoate | HCID 12463390 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3-Methyl-2-(propan-2-yl)butanenitrile | HCID 13699841 | 85% |
Reaction Steps
98.5 g (0.5 mol) of diisopropyl-cyanoacetic acid ethyl ester (prepared according to J. Chem. Soc., 1930, page 2,758), 300 ml of 1-oxo-1-methyl-phospholine, 31 g of sodium chloride and 22 g of water were heated to 160°-170° C. for 9 hours. After cooling, the mixture was diluted with 1,000 ml of water and extracted by shaking four times with 150 ml of petroleum ether each time. The combined petroleum ether phases were washed twice with 200 ml of water each time and dried with Na2SO4 and the petroleum ether was distilled off under normal pressure. The residual crude product was then purified by vacuum distillation. 53.2 g (85% of theory) of diisopropyl-acetonitrile of boiling point 60° C./14 mm Hg were obtained. Refractive index nD20 =1.4190.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04276225 |
| Source dataset | uspto-grants-1981_06 |
| ORD ID | ord-ee14cb9738184ddc95bd4954af833349 |
| Source note | uspto-grants-1981_06 |