2-Hydrazinopyridine → HCID 178515860, 화합물

HRID 476200

반응식

HRID 476200 반응식
O=[C:2]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH2:3][C:4]([O:6]CC)=O.[NH:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1)[NH2:17]>C(O)C>[CH2:9]([C:2]1[CH:3]=[C:4]([OH:6])[N:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[N:17]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

참가 물질

4

반응물 2

HCID 786452-HydrazinopyridineHCID 225855Ethyl 3-oxo-4-phenylbutanoate

생성물 1

HCID 178515860HCID 178515860, 화합물수율 30.8%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

Compound 2a (1.03 g, 5.0 mmol) prepared in Step 1 of Example A-1 was charged in a 25 mL round-bottom flask and dissolved in 6 mL of ethanol. A solution of 2-hydrazinopyridine (0.55 g, 5.0 mmol, manufactured by Aldrich) in 5 mL of ethanol at 50° C. was gradually added thereto over 30 minutes, followed by reaction for 1 hour. After completion of the reaction was confirmed by TLC, the reaction solution was concentrated by evaporation, extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated, and then purified by column chromatography [n-Hex/EtOAc=3/1 (v/v)] to afford a compound of 3-benzyl-1-(pyridin-2-yl)-1H-pyrazol-5-ol (3a).

후처리

  1. customfollowed by reaction for 1 hour
  2. concentrationthe reaction solution was concentrated by evaporation
  3. extractionextracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. custompurified by column chromatography [n-Hex/EtOAc=3/1 (v/v)]

출처 및 근거

ORD 기록
ord-8c28fcb7cca348d3bd20de67b4acdc17
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637674B2

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