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Acetone, oxime → 5-Acetyl-2-(2-chlorophenylamino)-3-fluoro-4-isopropylideneaminooxybenzoic acid methyl ester

HRID 917014
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HRID 917014 반응식
CC([O-])(C)C.[K+].[CH3:7][C:8](=[N:10][OH:11])[CH3:9].[CH3:12][O:13][C:14](=[O:34])[C:15]1[CH:20]=[C:19]([C:21](=[O:23])[CH3:22])[C:18](F)=[C:17]([F:25])[C:16]=1[NH:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[Cl:33]>C1COCC1>[CH3:12][O:13][C:14](=[O:34])[C:15]1[CH:20]=[C:19]([C:21](=[O:23])[CH3:22])[C:18]([O:11][N:10]=[C:8]([CH3:9])[CH3:7])=[C:17]([F:25])[C:16]=1[NH:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[Cl:33]
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참가 물질

5

반응물 3

HCID 67180Acetone, oximeHCID 23665647Potassium tert-butoxideHCID 865967735-Acetyl-2-(2-chlorophenylamino)-3,4-difluorobenzoic acid methyl ester

생성물 1

HCID 865967745-Acetyl-2-(2-chlorophenylamino)-3-fluoro-4-isopropylideneaminooxybenzoic acid methyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
-78 °C

실험 절차

t-BuOK (0.47 mL, 1.0 M in THF) was added to propan-2-one oxime (35 mg, 0.47 mmol). After stirring for 30 minutes, THF (0.5 mL) was added, and the reaction mixture was cooled to −78° C. A solution of 5-acetyl-2-(2-chlorophenylamino)-3,4-difluorobenzoic acid methyl ester (6) (50.0 mg, 0.147 mmol) in THF (1 mL) was added. The reaction mixture was slowly warmed to 0° C. and stirred for 2 hours. The reaction mixture was quenched with saturated aqueous NH4Cl, diluted with EtOAc and water. The aqueous layer was separated and extracted with EtOAc. The combined organic extracts were dried over MgSO4, filtered, and concentrated in vacuo to give the 5-acetyl-2-(2-chloro-phenylamino)-3-fluoro-4-isopropylideneaminooxy-benzoic acid methyl ester. The recovered oxime was suspended in a 1:1 mixture of 5% aqueous HCl and MeOH (30 ml) and heated to reflux. After 1 hour, the reaction mixture was cooled to room temperature and diluted with EtOAc. The organic layer was washed with water, dried (MgSO4) and concentrated. Purification by flash column chromatography using the Biotage system (40% methylene chloride in hexanes) provided 17 mg (35% for two steps) of the desired product (7).

후처리

  1. temperatureThe reaction mixture was slowly warmed to 0° C.
  2. stirringstirred for 2 hours
  3. customThe reaction mixture was quenched with saturated aqueous NH4Cl
  4. additiondiluted with EtOAc and water
  5. customThe aqueous layer was separated
  6. extractionextracted with EtOAc
  7. dry with materialThe combined organic extracts were dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-48a2fcb3be28451d8c4f485f259f1037
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07271178B2

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