Ammonium Chloride → N-(3-fluoro-4-(1-hydroxy-3-methyl-3-buten-1-yl)phenyl)pyridine-2-carboxamide

HRID 13426

反応式

HRID 13426 の反応式
[BH4-].[Na+].[F:3][C:4]1[CH:5]=[C:6]([NH:16][C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=2)=[O:18])[CH:7]=[CH:8][C:9]=1[C:10](=[O:15])[CH2:11][C:12]([CH3:14])=[CH2:13].[Cl-].[NH4+]>CO>[F:3][C:4]1[CH:5]=[C:6]([NH:16][C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=2)=[O:18])[CH:7]=[CH:8][C:9]=1[CH:10]([OH:15])[CH2:11][C:12]([CH3:14])=[CH2:13]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 4311764Sodium borohydrideHCID 23145243N-(3-fluoro-4-(3-methyl-3-butenoyl)phenyl)pyridine-2-carboxamide

生成物 1

HCID 23145600N-(3-fluoro-4-(1-hydroxy-3-methyl-3-buten-1-yl)phenyl)pyridine-2-carboxamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

88.8 mg of sodium borohydride was added to a methanol (5 ml) solution of 280 mg of N-(3-fluoro-4-(3-methyl-3-butenoyl)phenyl)pyridine-2-carboxamide. The reaction liquid was stirred at room temperature for 3 hours, and then poured into an aqueous saturated ammonium chloride solution, extracted with ethyl acetate, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=2/1) to obtain the entitled compound.

後処理

  1. customThe reaction liquid
  2. extractionextracted with ethyl acetate
  3. dry with materialdried with anhydrous sodium sulfate
  4. customThe solvent was evaporated away under reduced pressure
  5. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=2/1)
  6. customto obtain the entitled compound

出典と根拠

ORDレコード
ord-3f3cb1c020834c45a87b5331f0312cf0
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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