Acetic Acid → N-(2-cycloheptenyl)dichloromaleinimide

HRID 247620

Reaktionsgleichung

Reaktionsgleichung von HRID 247620
[CH:1]1([NH2:8])[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=[CH:2]1.[Cl:9][C:10]1=[C:11]([Cl:17])[C:12]([O:14][C:15]1=O)=[O:13].C(O)(=O)C>CCOCC>[CH:1]1([N:8]2[C:15](=[O:14])[C:10]([Cl:9])=[C:11]([Cl:17])[C:12]2=[O:13])[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=[CH:2]1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 70728Dichloromaleic anhydrideHCID 11263481Cyclohept-2-en-1-amine

Produkt 1

HCID 13578660N-(2-cycloheptenyl)dichloromaleinimideAusbeute 70,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A mixture of 2-cycloheptenylamine (1.01 g), dichloromaleic anhydride (1.67 g) and acetic acid (10 ml) was heated under reflux for 3 hours. After cooling, ether (20 ml) was added to the reaction mixture which was then washed with a saturated aqueous sodium hydrogencarbonate solution, water and a saturated aqueous sodium chloride solution in this order. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The deposited crystal was purified by recrystallization from hexane to obtain 1.67 g of N-(2-cycloheptenyl)dichloromaleinimide [Compound (217)].

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. temperatureAfter cooling
  4. washwas then washed with a saturated aqueous sodium hydrogencarbonate solution, water
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe deposited crystal was purified by recrystallization from hexane

Quellen und Nachweise

ORD-Eintrag
ord-abdfc592559a4f5aa99b7d586c93a409
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04709052

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