Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | 3,3-Dimethoxypropiononitrile | HCID 93731 | — |
| Reactant | HCID 70268884 | HCID 70268884 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water ethylacetate | HCID 22728543 | — |
| Product | HCID 86756097 | HCID 86756097 | — |
Reaction Steps
3,3-dimethoxy propionitrile (0.35 g, 0.0015×2 mol) was dissolved in a 2N aqueous hydrochloric acid solution (about 10 ml). The obtained solution was stirred at a temperature of about 50 to 60° C. for about one hour. The solution was further mixed with benzene (about 10 ml) and 4-methoxy-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide (0.50 g, 0.0015 mol), and then the resultant mixture was stirred at that temperature for about one hour. The obtained reaction solution was distributed in ethyl acetate-water The organic phase separated from the solution was successively washed with saturated sodium bicarbonate water and with saturated brine, and then dried with anhydrous sodium sulfate. Thereafter, the resultant solution was concentrated and then purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06159901 |
|---|
| Source dataset | uspto-grants-2000_12 |
|---|
| ORD ID | ord-39ae241fe19a48af9ac2212ae0e7915e |
|---|
| Source note | uspto-grants-2000_12 |
|---|