HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Chloro-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2.3,3,3-pentafluoropropylidene] hydrazide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 2776005 | HCID 2776005 | — |
| Reactant | 3-Chloro-6-[3-(trifluoromethyl)phenoxy]-picolinic acid hydrazide | HCID 70266266 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water ethylacetate | HCID 22728543 | — |
| Product | 3-Chloro-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2.3,3,3-pentafluoropropylidene] hydrazide | HCID 86756101 | — |
Reaction Steps
3-chloro-6-[3-(trifluoromethyl)phenoxy]-2-picolinic acid hydrazide (0.4 g, 0.0012 mol) was dissolved in 5 ml of acetic acid. The obtained solution was mixed with 2,2,3,3,3-pentafluoropropionaldehyde monohydrate (0.199 g, 0.0012×1.0 mol), and the resultant mixture was stirred at 80° C. for 3 hours. A chilled water was poured into the obtained reaction solution which was then distributed in ethyl acetate-water. The organic phase separated from the solution was washed with water and then dried with anhydrous sodium sulfate. After distilling off the solvent from the dried product, the obtained distillation residues were 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-f72fea7e3bc24759abbb7b8c7b4d054e |
| Source note | uspto-grants-2000_12 |