HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 5-Methoxy-4,4-dimethyl-3-oxopentanenitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl 3-methoxy-2,2-dimethylpropanoate | HCID 14302192 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 5-Methoxy-4,4-dimethyl-3-oxopentanenitrile | HCID 10898928 | — |
Reaction Steps
60% sodium hydride in mineral oil (667.2 mg, 16.68 mmol) in toluene (15 mL) is heated to reflux. A solution of 3-methoxy-2,2-dimethyl-propionic acid methyl ester (1.742 g, 11.916 mmol) and acetonitrile (0.878 mL, 16.68 mmol) in toluene (5 mL) is added dropwise through an additional funnel into the NaH suspension in toluene. After the addition, the reaction is stirred at reflux for 3 hours. After cooling, the reaction mixture is neutralized to PH˜7 by adding 1N HCl aqueous solution. The mixture is extracted with ethyl acetate 3 times. The organics are combined and washed with brine, dried over Na2SO4, filtered and concentrated in vacuo to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629157B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-d614fa2da10243d684cd0f6ca42c72bd |
| Source note | uspto-grants-2014_01 |