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Ethyl bromoacetate → 1-ethoxycarbonylmethyl-2,3-dihydro-1H-imidazo[1,2-b]pyrazole

HRID 2380287
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HRID 2380287 반응식
[NH:1]1[C:8]2[N:4]([N:5]=[CH:6][CH:7]=2)[CH2:3][CH2:2]1.Br[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12].C(=O)(O)[O-].[K+].C(OCC)(=O)C>CS(C)=O.O>[CH2:14]([O:13][C:11]([CH2:10][N:1]1[C:8]2[N:4]([N:5]=[CH:6][CH:7]=2)[CH2:3][CH2:2]1)=[O:12])[CH3:15]
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참가 물질

7

반응물 4

HCID 7748Ethyl bromoacetateHCID 8857Ethyl AcetateHCID 2424712,3-Dihydro-1H-imidazo(1,2-b)pyrazoleHCID 516893Potassium Bicarbonate

생성물 1

HCID 189552941-ethoxycarbonylmethyl-2,3-dihydro-1H-imidazo[1,2-b]pyrazole

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매
HCID 962
Water
용매

실험 절차

To a solution of 2,3-dihydro-1H-imidazo[1,2-b]-pyrazole (19 g) in dimethylsulfoxide (95 ml) were added ethyl bromoacetate (20.4 ml) and potassium bicarbonate (30 g) under ice-cooling. The mixture was stirred at room temperature for 4 hours. The reaction mixture was poured into a mixture of ethyl acetate (1.5 l) and water (500 ml). The separated organic layer was washed with water and brine, and dried over magnesium sulfate. The solvent was evaporated and the residue was subjected to column chromatography on silica gel using ethyl acetate as an eluent. Fractions containing the object compound were combined and evaporated in vacuo to give 1-ethoxycarbonylmethyl-2,3-dihydro-1H-imidazo[1,2-b]pyrazole (20.3 g).

후처리

  1. temperaturecooling
  2. washThe separated organic layer was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated
  5. additionFractions containing the object compound
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-b1aa8e6d07a0421ca12b5c590f597c0a
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05366970

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