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Water → 1-(2-hydroxyethyl)-2,3-dihydro-1H-imidazo[1,2-b]pyrazole

HRID 1681655
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HRID 1681655 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:9][C:10]([CH2:12][N:13]1[C:20]2[N:16]([N:17]=[CH:18][CH:19]=2)[CH2:15][CH2:14]1)=O)C.[F-].[Na+].O>O1CCCC1>[OH:9][CH2:10][CH2:12][N:13]1[C:20]2[N:16]([N:17]=[CH:18][CH:19]=2)[CH2:15][CH2:14]1
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참가 물질

6

반응물 4

HCID 962WaterHCID 5235Sodium FluorideHCID 189552941-ethoxycarbonylmethyl-2,3-dihydro-1H-imidazo[1,2-b]pyrazoleHCID 21226445Aluminium lithium hydride

생성물 1

HCID 150777341-(2-hydroxyethyl)-2,3-dihydro-1H-imidazo[1,2-b]pyrazole수율 37.7%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

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온도
50 °C

실험 절차

To a suspension of lithium aluminum hydride (3.89 g) in tetrahydrofuran (195 ml) was added dropwise a solution of 1-ethoxycarbonylmethyl-2,3-dihydro-1H-imidazo[1,2-b]-pyrazole (20 g) in tetrahydrofuran (100 ml) at room temperature. The mixture was stirred at 50° C. for 1 hour. The reaction mixture was cooled under ice-bath To a mixture were added sodium fluoride (17.2 g) and water (5.5 ml) under ice-cooling. The insoluble material was filtered off and the filtrate was evaporated. 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-(2-hydroxyethyl)-2,3-dihydro-1H-imidazo[1,2-b]pyrazole (5.91 g).

후처리

  1. temperatureThe reaction mixture was cooled under ice-bath To a mixture
  2. temperaturecooling
  3. filtrationThe insoluble material was filtered off
  4. customthe filtrate was evaporated
  5. additionFractions containing the object compound
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-75e67cb050694618b9c3a0c5462c1b7d
출처 데이터셋
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05173485

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