Sodium Hydroxide → Chlorazifop

HRID 249199노트

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HRID 249199 반응식
[OH-].[Na+].[Cl:3][C:4]1[C:5]([O:11][C:12]2[CH:25]=[CH:24][C:15]([O:16][CH:17]([CH3:23])[C:18]([O:20]CC)=[O:19])=[CH:14][CH:13]=2)=[N:6][CH:7]=[C:8]([Cl:10])[CH:9]=1>O1CCCC1>[Cl:3][C:4]1[C:5]([O:11][C:12]2[CH:13]=[CH:14][C:15]([O:16][CH:17]([CH3:23])[C:18]([OH:20])=[O:19])=[CH:24][CH:25]=2)=[N:6][CH:7]=[C:8]([Cl:10])[CH:9]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 2829855Propanoic acid, 2-[4-[(3,5-dichloro-2-pyridinyl)oxy]phenoxy]-, ethyl ester

생성물 1

HCID 173715Chlorazifop수율 70%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
52 °C

실험 절차

10% Sodium hydroxide solution (170 mL, 0.424 mol) is added to a solution of ethyl 2-{p-[(3,5-dichloro-2-pyridyl)oxy]phenoxy}propionate (79.09 g, 0.212 mol) in tetrahydrofuran with stirring. The reaction mixture is heated to 52° C., stirred for 3 hours, concentrated in vacuo and diluted with water. The aqueous solution is washed with methylene chloride, acidified with concentrated sulfuric acid and extracted with ethyl acetate. The combined organic extracts are dried and concentrated in vacuo to give the title product as a white solid (48.7 g) which is identified by 1H NMR spectral analysis.

후처리

  1. stirringstirred for 3 hours
  2. concentrationconcentrated in vacuo
  3. additiondiluted with water
  4. washThe aqueous solution is washed with methylene chloride
  5. extractionextracted with ethyl acetate
  6. customThe combined organic extracts are dried
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3ccf186c65be463b818d6c1b2de5565f
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05213606

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