Water → HCID 14625291、化合物

HRID 1073677ノート

反応式

HRID 1073677 の反応式
[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

参加物

6

反応物 4

HCID 962WaterHCID 81882Butyl GlycolateHCID 522689Potassium FluorideHCID 14625290HCID 14625290、化合物

生成物 1

HCID 14625291HCID 14625291、化合物収率 75.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e420d9b7d1874a5db31ea6443ee79659
出典データセット
uspto-grants-1990_11
特許番号
US04970322

反応ノート

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