Diethyl (1-methylpropyl)malonate → HCID 21272884, Verbindung

HRID 1382660

Reaktionsgleichung

Reaktionsgleichung von HRID 1382660
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH2:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[CH:11]([CH:15]([C:21](OCC)=[O:22])[C:16](OCC)=[O:17])([CH2:13][CH3:14])[CH3:12]>>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:16](=[O:17])[CH:15]([CH:11]([CH2:13][CH3:14])[CH3:12])[C:21](=[O:22])[NH:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

Komponenten

3

Edukt 2

HCID 78940Diethyl (1-methylpropyl)malonateHCID 83161(3,4-Dichlorophenyl)hydrazine

Produkt 1

HCID 21272884HCID 21272884, VerbindungAusbeute 76,2 %

Versuchsvorschrift

50 g of 3,4-dichlorophenylhydrazine (85%) and 122.5 g of diethyl sec-butyl-malonate were heated for 10 hours at 180° C. (external temperature) while distilling 21.3 g of ethanol. The remainder was taken up in 200 ml of methylene chloride, and the solution was extracted with 2N sodium hydroxide, then with water. The combined aqueous phases were washed with methylene chloride and acidified to pH 1 by concentrated hydrochloric acid. The precipitate was separated, washed with water, separated, dried under reduced pressure at 40° C. to obtain 64.8 g of 1-(3,4-dichlorophenyl)-4-(sec-butyl)-pyrazolidine-3,5-dione melting at 118°-120° C.

Aufarbeitung

  1. distillationwhile distilling 21.3 g of ethanol
  2. extractionthe solution was extracted with 2N sodium hydroxide
  3. washThe combined aqueous phases were washed with methylene chloride
  4. customThe precipitate was separated
  5. washwashed with water
  6. customseparated
  7. customdried under reduced pressure at 40° C.

Quellen und Nachweise

ORD-Eintrag
ord-96d0074933c341588da4dcaf1c95ccfc
Quelldatensatz
uspto-grants-1989_02
Patentnummer
US04808210

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