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

HRID 1781118
ノート
印刷プレビュー

反応式

HRID 1781118 の反応式
[N:1]12[CH2:8][CH2:7][N:4]([CH2:5][CH2:6]1)[CH2:3][CH2:2]2.OO.N12CC[N+]([O-])(CC1)CC2.[C:20](Cl)(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[F:29][B-:30]([F:33])([F:32])[F:31].[Na+]>C1COCC1.C(#N)C>[F:29][B-:30]([F:33])([F:32])[F:31].[C:20]([N+:1]12[CH2:8][CH2:7][N:4]([CH2:5][CH2:6]1)[CH2:3][CH2:2]2)(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 784Hydrogen PeroxideHCID 7412Benzoyl chlorideHCID 9237DabcoHCID 4343483Sodium TetrafluoroborateHCID 111371811,4-Diazabicyclo(2.2.2)octane, 1-oxide

生成物 1

HCID 190480521-Benzoyl-4-aza-1-azoniabicyclo[2.2.2]octane tetrafluoroborate

試薬・触媒・溶媒 2

HCID 6342
Acetonitrile
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

1-benzoyl-4-fluoro-1,4-diazoniabicvclo[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 mmool) in THF (100 mL) is reacted with benzoyl chloride (14 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 filtrate is evaporated to afford 1-benzoyl-4-aza-1-azoniabicyclo[2.2.2]octane tetrafluoroborate.

後処理

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

出典と根拠

ORDレコード
ord-25a11841b6164cf5bb6272caa2ef15ea
出典データセット
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05631372

反応ノート

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