4-Morpholinobenzonitrile → 4-Morpholinobenzylamine

HRID 585994

反応式

HRID 585994 の反応式
[N:1]1([C:7]2[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][CH:8]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[N:1]1([C:7]2[CH:8]=[CH:9][C:10]([CH2:11][NH2:12])=[CH:13][CH:14]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 3948084-MorpholinobenzonitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 27764584-Morpholinobenzylamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4-(4-Morpholinyl)benzonitrile (1.24 g, 6.6 mmol) in THF (25 mL) at 0° C. was treated with LiAlH4 (2.5 g, 65.9 mmol) and refluxed for 1 hour. The mixture was cooled to room temperature and quenched by careful addition of 1N NaOH and then H2O. The mixture was concentrated, extracted with diethyl ether. The combined ethereal extracts were washed with saturated NaHCO3 solution, dried over Na2SO4, and evaporated in vacuo to provide the title compound which was dried over MgSO4 as a THF:diethylether solution before the next step.

後処理

  1. temperaturerefluxed for 1 hour
  2. customquenched by careful addition of 1N NaOH
  3. concentrationThe mixture was concentrated
  4. extractionextracted with diethyl ether
  5. washThe combined ethereal extracts were washed with saturated NaHCO3 solution
  6. dry with materialdried over Na2SO4
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-979ec15a92dc408899029fd55e65e1d4
出典データセット
uspto-grants-2005_08
特許番号
US06933311B2

関連ノート

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