Water → 4-Methyl-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2,3,3,3-pentafluoropropylidene] hydrazide

HRID 1274819노트

반응식

HRID 1274819 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=2)[N:5]=[C:4]([C:19]([NH:21][NH2:22])=[O:20])[CH:3]=1.O.[F:24][C:25]([F:32])([C:28]([F:31])([F:30])[F:29])[CH:26]=O.O>C(O)(=O)C.C(OCC)(=O)C.O>[F:24][C:25]([F:32])([C:28]([F:31])([F:30])[F:29])[CH:26]=[N:22][NH:21][C:19](=[O:20])[C:4]1[CH:3]=[C:2]([CH3:1])[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:16])([F:17])[F:18])[CH:10]=2)[N:5]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 2776005HCID 2776005, 화합물HCID 702663564-Methyl-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide

생성물 1

HCID 867561034-Methyl-6-[3-(trifluoromethyl)phenoxy] picolinic acid, (2,2,3,3,3-pentafluoropropylidene] hydrazide

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 22728543Water ethylacetate용매

실험 절차

4-methyl-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide (0.38 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 (0.40 g, 0.0012×2 mol), and then the resultant mixture was stirred at 80° C. for 3 hours. Thereafter, 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.

후처리

  1. customThe organic phase separated from the solution
  2. washwas washed with water
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationAfter distilling off the solvent from the dried product
  5. distillationthe obtained distillation residues
  6. customwere purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-0bf79456acdb40a98c2c28553da89a33
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06159901

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