Sodium Hydroxide → Endo-3,9-dimethyl-3,9-diazabicyclo[3.3.1)nonan-7-ol

HRID 1656912ノート

反応式

HRID 1656912 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[O:7]=[C:8]1[CH2:15][CH:14]2[N:16]([CH3:17])[CH:10]([CH2:11][N:12]([CH3:18])[CH2:13]2)[CH2:9]1.[OH-].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>C1COCC1.O>[CH3:18][N:12]1[CH2:11][CH:10]2[N:16]([CH3:17])[CH:14]([CH2:15][CH:8]([OH:7])[CH2:9]2)[CH2:13]1

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 197864093,9-Dimethyl-3,9-diazabicyclo[3.3.1]nonan-7-oneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 19786410Endo-3,9-dimethyl-3,9-diazabicyclo[3.3.1)nonan-7-ol収率 93.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of lithium aluminum hydride (0.95 g, 25.0 mmol) in dry THF (40 ml) was added dropwise at room temperature while stirring a solution of 7-oxo-3,9-dimethyl3,9-diazabicyclo[3.3.1)nonane (2.78 g, 16.5 mmol) in dry THF (50 ml). After stirring at room temperature for 4.5 hrs, water (1 ml), 40% aqueous sodium hydroxide solution (1 ml) and water (3 ml) were added successively to a reaction solution. Further anhydrous magnesium sulfate was added and stirred, and thereafter the reaction was filtered. The filtrate was concentrated under reduced pressure to afford the title compound (2.62 g) as an oily product.

後処理

  1. additionwas added dropwise at room temperature
  2. stirringstirred
  3. filtrationthe reaction was filtered
  4. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-a16bbbad821e42aca73bc72d77918aa5
出典データセット
uspto-grants-1993_10
特許番号
US05256656

反応ノート

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