Hydrogen Peroxide → 1-Acetoxy-4-aza-1-azoniabicyclo[2.2.2]octane tetrafluoroborate

HRID 1781116노트

반응식

HRID 1781116 반응식
N12CCN(CC1)CC2.OO.[N:11]12[CH2:18][CH2:17][N+:14]([O-:19])([CH2:15][CH2:16]1)[CH2:13][CH2:12]2.[C:20](Cl)(=[O:22])[CH3:21].[F:24][B-:25]([F:28])([F:27])[F:26].[Na+]>C1COCC1.C(#N)C>[N:11]12[CH2:18][CH2:17][N+:14]([O-:19])([CH2:15][CH2:16]1)[CH2:13][CH2:12]2.[F:24][B-:25]([F:28])([F:27])[F:26].[F:24][B-:25]([F:28])([F:27])[F:26].[C:20]([O:19][N+:14]12[CH2:17][CH2:18][N+:11]([F:24])([CH2:16][CH2:15]1)[CH2:12][CH2:13]2)(=[O:22])[CH3:21].[F:24][B-:25]([F:28])([F:27])[F:26].[C:20]([O:19][N+:14]12[CH2:17][CH2:18][N:11]([CH2:16][CH2:15]1)[CH2:12][CH2:13]2)(=[O:22])[CH3:21]

참가 물질

9

반응물 5

HCID 784Hydrogen PeroxideHCID 6367Acetyl chlorideHCID 9237DabcoHCID 4343483Sodium TetrafluoroborateHCID 111371811,4-Diazabicyclo(2.2.2)octane, 1-oxide

생성물 2

HCID 190480361-Acetoxy-4-aza-1-azoniabicyclo[2.2.2]octane tetrafluoroborateHCID 867508561-acetoxy-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) 1,4-Diazabicyclo[2.2.2]octane N-oxide

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매

실험 절차

1-acetoxy-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) 1,4-Diazabicyclo[2.2.2]octane N-oxide is prepared by the reaction of 1,4-diazabicyclo[2.2.2]octane with hydrogen peroxide as described by Farkas in J. Chem. Eng. Data (1968) 13,278. 1,4-Diazabicyclo[2.2.2]octane N-oxide (12.8 g, 10 mmol) in THF (100 mL) is reacted with acetyl chloride (7.9 g, 10 mmol) until the reaction is complete by TLC. The reaction is evaporated, diluted with acetonitrile (100 mL) and sodium tetrafluoroborate (40 g, 20 mmol) added. The solution is stirred overnight at room temperature and then filtered to remove all undissolved salts. The flltrate is evaporated to afford 1-acetoxy-4-aza-1-azoniabicyclo[2.2.2]octane tetrafluoroborate.

후처리

  1. customThe reaction is evaporated
  2. additionadded
  3. filtrationfiltered
  4. customto remove all undissolved salts
  5. customThe flltrate is evaporated

출처 및 근거

ORD 기록
ord-f9e0c9f2c0c944d59a70ae8393a741c1
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05631372

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