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

HRID 13426

반응식

HRID 13426 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3f3cb1c020834c45a87b5331f0312cf0
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

연결된 노트

불러오는 중…