Perchloric Acid → HCID 21998067, Verbindung

HRID 1977444Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1977444
[O:1]1[CH2:18][CH:2]1[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:15](=[O:16])[CH:14]=[CH:13][C:12]2=[O:17])=[CH:7][CH:6]=1.Cl(O)(=O)(=O)=[O:20].ClCCl.CO>CC(C)=O.O>[OH:20][CH:2]([CH2:18][OH:1])[CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C:12](=[O:17])[CH:13]=[CH:14][C:15]2=[O:16])=[CH:9][CH:10]=1

Komponenten

6

Edukt 3

HCID 24247Perchloric AcidHCID 21226129Dichloromethane methanolHCID 219980621H-Pyrrole-2,5-dione, 1-[4-(oxiranylmethoxy)phenyl]-

Produkt 1

HCID 21998067HCID 21998067, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a suspension of N-(4-[2,3-epoxypropyl]oxyphenyl)maleimide (200 g, 0.816 mole) in 1360 ml of acetone was added perchloric acid (20 ml) in 660 ml of water. The reaction mixture was refluxed for 2 h, during which the solution became clear yellow (complete conversion on TLC, dichloromethane: methanol 90:10). After cooling, the acetone was removed under reduced pressure. Water was added to the resulting slurry which was stirred for 0.5 h. The solids were filtered off, washed with water and dissolved in THF (tetrahydrofuran). This solution was dried twice over anhydrous sodium sulfate, followed by concentration to dryness.

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 2 h, during which the solution
  2. temperatureAfter cooling
  3. customthe acetone was removed under reduced pressure
  4. additionWater was added to the resulting slurry which
  5. filtrationThe solids were filtered off
  6. washwashed with water
  7. dissolutiondissolved in THF (tetrahydrofuran)
  8. dry with materialThis solution was dried twice over anhydrous sodium sulfate
  9. concentrationfollowed by concentration to dryness

Quellen und Nachweise

ORD-Eintrag
ord-0423c2c9f6b54f89a41049d9c0568e20
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06232430B1

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