Dichloroacetyl chloride → N-dichloroacetylpiperid-4-one ethylene ketal

HRID 65387

Reaktionsgleichung

Reaktionsgleichung von HRID 65387
[Cl:1][CH:2]([Cl:6])[C:3](Cl)=[O:4].[CH2:7]1[O:16][C:10]2([CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[O:9][CH2:8]1>C1(C)C=CC=CC=1>[CH2:7]1[O:16][C:10]2([CH2:15][CH2:14][N:13]([C:3](=[O:4])[CH:2]([Cl:6])[Cl:1])[CH2:12][CH2:11]2)[O:9][CH2:8]1

Komponenten

4

Edukt 2

HCID 6593Dichloroacetyl chlorideHCID 674351,4-Dioxa-8-azaspiro(4.5)decane

Produkt 1

HCID 13018227N-dichloroacetylpiperid-4-one ethylene ketalAusbeute 49,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

12.4 g (0.084 mol) of dichloroacetyl chloride was added dropwise to a mixture of 12 g (0.084 mol) of piperid-4-one ethylene ketal and 12.8 g (0.084 mol) of 1,8-diazobicyclo[5.4.0]undec-7-ene in 100 ml of toluene, whilst stirring, at a rate such that the temperature of the reaction mixture did not exceed 40° C. Thereafter, the mixture was subsequently stirred at 20° C. for 2 hours. Working up was then effected by a procedure in which the reaction mixture was filtered, the filtrate was concentrated under reduced pressure and the residue was recrystallized from a mixture of toluene and petroleum ether. 10.5 g (49% of theory) of N-dichloroacetylpiperid-4-one ethylene ketal were obtained in this manner in the form of colorless crystals of melting point 102° C.

Aufarbeitung

  1. customdid not exceed 40° C
  2. stirringThereafter, the mixture was subsequently stirred at 20° C. for 2 hours
  3. filtrationwas filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customthe residue was recrystallized from a mixture of toluene and petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-8cc022afb8cb4deeb6634dc0ea0dc597
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04614537

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