Hydrazine hydrate (1:1) → 3-Chloro-6-[3-(trifluoromethyl)phenoxy]-picolinic acid hydrazide

HRID 1274826ノート

反応式

HRID 1274826 の反応式
C[O:2][C:3](=O)[C:4]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[N:5]=1.O.[NH2:24][NH2:25]>CO>[Cl:10][C:9]1[C:4]([C:3]([NH:24][NH2:25])=[O:2])=[N:5][C:6]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 539496273-Chloro-6-[3-(trifluoromethyl)phenoxy]-2-picolinic acid methyl ester

生成物 1

HCID 702662663-Chloro-6-[3-(trifluoromethyl)phenoxy]-picolinic acid hydrazide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-chloro-6- [3-(trifluoromethyl)phenoxy]-2-picolinic acid methyl ester (0.72 g, 0.00217 mol) was dissolved in methanol (10 ml), and then mixed with hydrazine monohydrate (1.087 g, 0.00217×10 mol). The resultant mixture was refluxed for about 3 hours. The obtained reaction solution was concentrated, and the obtained residues were distributed in ethyl acetate-saturated sodium bicarbonate water. The organic phase separated from the solution was washed with water and then dried with anhydrous sodium sulfate. After distilling off the solvent, 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 obtained reaction solution
  2. concentrationwas concentrated
  3. customThe organic phase separated from the solution
  4. washwas washed with water
  5. dry with materialdried with anhydrous sodium sulfate
  6. distillationAfter distilling off the solvent
  7. distillationthe obtained distillation residues
  8. customwere purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-75954316e9554ebfbfb0f8a019c11420
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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