Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-Butyn-1-al diethyl acetal | HCID 137721 | — |
| Reactant | HCID 70268884 | HCID 70268884 | — |
| Solvent | Water ethylacetate | HCID 22728543 | — |
| Product | HCID 86756104 | HCID 86756104 | — |
Reaction Steps
2-butyne-1-al diethyl acetal (0.27 g, 0.000993×2 mol) was mixed with a 2N aqueous hydrochloric acid solution (about 3 ml) and 5 ml of benzene, and then the resultant mixture was stirred at about 70° C. for about 2 hours. After cooling to room temperature, the obtained mixture was mixed with 4-methoxy-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide (0.325 g, 0.000993 mol), and the resultant mixture was stirred at room temperature for 45 minutes. The obtained reaction solution was distributed in ethyl acetate-water, and the organic phase separated from the solution was washed with saturated brine, dried with anhydrous sodium sulfate and then concentrated. The obtained concentrated solution was 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 |
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| Patent number | US06159901 |
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| Source dataset | uspto-grants-2000_12 |
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| ORD ID | ord-08de3bf501d64b6e8d5c465ebbe5526a |
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| Source note | uspto-grants-2000_12 |
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