Water → HCID 14625291, 화합물

HRID 1073677노트

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HRID 1073677 반응식
[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([N+:17]([O-:19])=[O:18])[C:14](F)=[CH:13][C:12]=2[F:21])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2.[CH3:22][CH2:23][CH2:24][CH2:25][O:26][C:27]([CH2:29][OH:30])=[O:28].[F-].[K+].O>O1CCOCC1>[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([N+:17]([O-:19])=[O:18])[C:14]([O:30][CH2:29][C:27]([O:26][CH2:25][CH2:24][CH2:23][CH3:22])=[O:28])=[CH:13][C:12]=2[F:21])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

참가 물질

6

반응물 4

HCID 962WaterHCID 81882Butyl GlycolateHCID 522689Potassium FluorideHCID 14625290HCID 14625290, 화합물

생성물 1

HCID 14625291HCID 14625291, 화합물수율 75.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A suspension of 3-chloro-2-(2,4-difluoro-5-nitrophenyl)-4,5,6,7-tetrahydro-2H-indazole (10 g), butyl glycollate (5 g) and potassium fluoride (10 g) in dioxane (30 g) was refluxed for 1 hour. After completion of the reaction, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated. The residue was purified by liquid column chromatography using a mixture of hexane and ethyl acetate as an eluent to give 3-chloro-2-(2-fluoro-4-butyloxycarbonylmethoxy-5-nitro-phenyl)-4,5,6,7-tetrahydro-2H-indazole (10.2 g). m.p., 138°-139° C.

후처리

  1. temperaturewas refluxed for 1 hour
  2. customAfter completion of the reaction
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by liquid column chromatography
  7. additiona mixture of hexane and ethyl acetate as an eluent

출처 및 근거

ORD 기록
ord-e420d9b7d1874a5db31ea6443ee79659
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04970322

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