Aluminium lithium hydride → HCID 71744071、化合物

HRID 869477ノート

反応式

HRID 869477 の反応式
[N:1]1[CH:2]=[C:3]([C:10](OCC)=[O:11])[N:4]2[C:9]=1[CH:8]=[CH:7][CH:6]=[N:5]2.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[N:1]1[CH:2]=[C:3]([CH2:10][OH:11])[N:4]2[C:9]=1[CH:8]=[CH:7][CH:6]=[N:5]2

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 71744070Ethyl imidazo[1,2-B]pyridazine-3-carboxylate

生成物 1

HCID 71744071HCID 71744071、化合物収率 57%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl imidazo[1,2-b]pyridazine-3-carboxylate (1.91 g, 10 mmol) in anhydrous THF (20 mL), lithium aluminium hydride (1.34 g, 35 mmol) was added in portions over 15 min. After stirring at RT for 16 h, the mixture was quenched with ice-water (20 mL) and then extracted with ethyl acetate (30 mL×2). The combined organic layers were washed with brine, dried over Na2SO4 then filtered. The filtrate was concentrated in vacuo to afford imidazo[1,2-b]pyridazin-3-ylmethanol (0.85 g, 57% yield).

後処理

  1. customthe mixture was quenched with ice-water (20 mL)
  2. extractionextracted with ethyl acetate (30 mL×2)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationthen filtered
  6. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-4afacf5250e445019a0d7611ee1548d6
出典データセット
uspto-grants-2015_03
特許番号
US08969363B2

反応ノート

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