HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-(1-Methylpiperidin-4-ylidene)acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Methyl-4-piperidone | HCID 74049 | — |
| Reactant | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(1-Methylpiperidin-4-ylidene)acetonitrile | HCID 21825020 | — |
Reaction Steps
9.36 g of K2CO3 and 8.89 ml of diethyl (cyanomethyl)phosphonate are placed in 12 ml of THF in a round-bottomed flask equipped with a magnetic stirrer, and under a stream of nitrogen, and the mixture is left to react for 15 minutes at room temperature and then refluxed for 20 minutes. The resulting mixture is allowed to cool and 6.5 ml of 1-methyl-4-piperidone are added dropwise. This mixture is refluxed for 16 hours. The reaction mixture is then poured into water and extracted with ethyl acetate. The organic phase is dried over Na2SO4, filtered and evaporated under vacuum. 6.8 g of oil are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08202871B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-85c01a36266d4b579c83c44afc59a619 |
| Source note | uspto-grants-2012_06 |