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Water → 1-(2-Pyrimidinyl)-4-piperidinemethanol

HRID 1485108
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HRID 1485108 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][OH:8])[CH2:3][CH2:2]1.Cl[C:10]1[N:15]=[CH:14][CH:13]=[CH:12][N:11]=1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O.C(OCC)(=O)C>[N:11]1[CH:12]=[CH:13][CH:14]=[N:15][C:10]=1[N:1]1[CH2:6][CH2:5][CH:4]([CH2:7][OH:8])[CH2:3][CH2:2]1
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참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 744042-ChloropyrimidineHCID 4207714-Piperidinemethanol

생성물 1

HCID 27765211-(2-Pyrimidinyl)-4-piperidinemethanol수율 89.4%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매
HCID 8857
Ethyl Acetate
용매

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온도
100 °C

실험 절차

To a solution of 4-piperidinemethanol (1.00 g) in dimethyl sulfoxide (28.9 mL), 2-chloropyrimidine (994 mg) and potassium carbonate (2.40 g) were added and the mixture was stirred at 100° C. for three hours. After cooling the reaction mixture to room temperature, water was added to it and extraction was conducted with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and after removing the desiccant by filtration, the filtrate was concentrated under reduced pressure to give [1-([pyrimidin-2-yl)piperidin-4-yl]methanol as a colorless oil (1.50 g).

후처리

  1. temperatureAfter cooling the reaction mixture to room temperature
  2. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  3. customafter removing the
  4. filtrationdesiccant by filtration
  5. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a1999d9a8d8c4eabbe8845792a9825cc
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422240B2

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