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

HRID 2380288
ノート
印刷プレビュー

反応式

HRID 2380288 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

反応条件

温度
50 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-6796db5375a0432db7d06f8cbf4e62fc
出典データセット
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05366970

反応ノート

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