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

HRID 1656912노트

반응식

HRID 1656912 반응식
[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

참가 물질

7

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-a16bbbad821e42aca73bc72d77918aa5
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05256656

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