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

HRID 1274819ノート

反応式

HRID 1274819 の反応式
[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

参加物

6

反応物 3

HCID 962WaterHCID 2776005HCID 2776005、化合物HCID 702663564-Methyl-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 22728543Water ethylacetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-0bf79456acdb40a98c2c28553da89a33
出典データセット
uspto-grants-2000_12
特許番号
US06159901

反応ノート

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