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

HRID 1781116ノート

反応式

HRID 1781116 の反応式
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]

参加物

9

反応物 5

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

生成物 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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f9e0c9f2c0c944d59a70ae8393a741c1
出典データセット
uspto-grants-1997_05
特許番号
US05631372

反応ノート

読み込み中…