Dichloromethane → HCID 86699684, Verbindung

HRID 1487192

Reaktionsgleichung

Reaktionsgleichung von HRID 1487192
Cl[C:2]1[CH:3]=[CH:4][C:5]([N+:13]([O-:15])=[O:14])=[C:6]([CH:8]2[O:12][CH2:11][CH2:10][O:9]2)[CH:7]=1.ClCCl.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1>>[O:9]1[CH2:10][CH2:11][O:12][CH:8]1[C:6]1[CH:7]=[C:2]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[CH:3]=[CH:4][C:5]=1[N+:13]([O-:15])=[O:14]

Komponenten

4

Edukt 3

HCID 6344DichloromethaneHCID 8083MorpholineHCID 2673852-(5-Chloro-2-nitrophenyl)-1,3-dioxolane

Produkt 1

HCID 86699684HCID 86699684, VerbindungAusbeute 97,1 %

Versuchsvorschrift

2-(5-Chloro-2-nitrophenyl)-1,3-dioxolane (13.4 g, 58.4 mmol) was dissolved in morpholine (150 mL). The mixture was then heated to reflux for 16 hours. Cooling to room temperature, dichloromethane was added. The organic phase was washed with water, dried over anhydrous sodium sulfate, evaporated and purified by silica gel chromatography to afford the product 4-(3-(1,3-dioxolan-2-yl)-4-nitrophenyl)morpholine (15.9 g, yield 97.1%).

Aufarbeitung

  1. temperatureThe mixture was then heated
  2. temperatureto reflux for 16 hours
  3. washThe organic phase was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. custompurified by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-4a084a21f93a422d9e51761a639bc4a8
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09428508B2

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