1,4-Diazabicyclo(3.2.2)nonan-3-one → 1,4-Diazabicyclo(3.2.2)nonane

HRID 867502

반응식

HRID 867502 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].O=[C:8]1[NH:14][CH:13]2[CH2:15][CH2:16][N:10]([CH2:11][CH2:12]2)[CH2:9]1>O1CCCC1>[N:10]12[CH2:16][CH2:15][CH:13]([CH2:12][CH2:11]1)[NH:14][CH2:8][CH2:9]2

참가 물질

4

반응물 2

HCID 44018501,4-Diazabicyclo(3.2.2)nonan-3-oneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 3984071,4-Diazabicyclo(3.2.2)nonane수율 64.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium aluminum hydride (2.0 g, 51.4 mmoles) was slurried in 250 ml of dry tetrahydrofuran and 3-oxo-1,4-diazabicyclo[3.2.2]nonane (3.6 g, 25.7 mmoles) was added carefully as a solid in one portion at room temperature. The resulting mixture was then heated to a gentle reflux for 20 hours. The reaction was cooled to room tempeature and quenched by slow addition of 2.5 ml water. The salts were filtered and washed several times with diethyl ether totaling 1.0 1. These washings and the supernatant were combined, dried over magnesium sulfate and concentrated to give 2.09 g (64.5%) of the title compound as a pale yellow oil.

후처리

  1. temperatureThe resulting mixture was then heated to
  2. temperaturea gentle reflux for 20 hours
  3. temperatureThe reaction was cooled to room tempeature
  4. customquenched by slow addition of 2.5 ml water
  5. filtrationThe salts were filtered
  6. washwashed several times with diethyl ether totaling 1.0 1
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c29499e62b974f038a1fcb19a31047d6
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04775668

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