Water → HCID 19068987, Verbindung

HRID 1735094Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1735094
[CH3:1][N:2]1[C:12]2[C:7](=[C:8]([Cl:14])[CH:9]=[C:10]([Cl:13])[CH:11]=2)[C:5](=O)[C:3]1=[O:4].NN.[Na].O>C(O)C>[CH3:1][N:2]1[C:12]2[C:7](=[C:8]([Cl:14])[CH:9]=[C:10]([Cl:13])[CH:11]=2)[CH2:5][C:3]1=[O:4]

Komponenten

6

Edukt 4

HCID 962WaterHCID 9321HydrazineHCID 5360545SodiumHCID 185185371-Methyl-4,6-dichloroisatin

Produkt 1

HCID 19068987HCID 19068987, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

1-Methyl-4,6-dichloroisatin (4.0 g) was suspended in dry ethanol (40 ml), hydrazine (9 ml) was added and the mixture was refluxed in 6 h. The mixture was then added slowly at 70° C. to a solution of sodium (1.74 g)in dry ethanol (80 ml) and refluxed overnight. The reaction mixture was cooled to room temperature, water (50 ml) was added and the volume was reduced to about one third by evaporation. The mixture was then poured onto icewater (1000 ml) and acidified with 6M HCl (pH=1). The precipitate was filtered off washed with water and dried to afford 3.27 g (87%) of (43). M.p. 144°-145° C.

Aufarbeitung

  1. temperaturethe mixture was refluxed in 6 h
  2. temperaturerefluxed overnight
  3. customthe volume was reduced to about one third by evaporation
  4. additionThe mixture was then poured onto icewater (1000 ml)
  5. filtrationThe precipitate was filtered off
  6. washwashed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3526e775dc8949c189de3b95f5bcccbf
Quelldatensatz
uspto-grants-1996_07
Patentnummer
US05536721

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