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

HRID 1274826노트

반응식

HRID 1274826 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-75954316e9554ebfbfb0f8a019c11420
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06159901

반응 노트

불러오는 중…