Acetic Anhydride → HCID 54074224, Verbindung

HRID 1763169Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1763169
[C:1]([O:4][C:5](=O)[CH3:6])(=O)[CH3:2].[CH2:8]([O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]([C:19]2[CH:24]=[CH:23][C:22]([N:25]([CH3:27])[CH3:26])=[CH:21][CH:20]=2)=[CH2:18])=[CH:13][CH:12]=1)[CH3:9].[Cl:28][C:29]1[C:30]([Cl:42])=[C:31]([Cl:41])[C:32]([Cl:40])=[C:33]2[C:38](=O)[O:37][C:35](=[O:36])[C:34]=12.[OH-].[Na+]>O.ClC1C=CC=CC=1Cl>[CH3:27][N:25]([CH3:26])[C:22]1[CH:21]=[CH:20][C:19]([C:17]([C:14]2[CH:15]=[CH:16][C:11]([O:10][CH2:8][CH3:9])=[CH:12][CH:13]=2)=[CH:18][C:38]2([CH:18]=[C:17]([C:14]3[CH:13]=[CH:12][C:1]([O:4][CH2:5][CH3:6])=[CH:2][CH:15]=3)[C:19]3[CH:24]=[CH:23][C:22]([N:25]([CH3:27])[CH3:26])=[CH:21][CH:20]=3)[C:33]3[C:34](=[C:29]([Cl:28])[C:30]([Cl:42])=[C:31]([Cl:41])[C:32]=3[Cl:40])[C:35](=[O:36])[O:37]2)=[CH:24][CH:23]=1

Komponenten

7

Edukt 4

HCID 7918Acetic AnhydrideHCID 8326Tetrachlorophthalic anhydrideHCID 14798Sodium HydroxideHCID 145122554-[1-(4-Ethoxyphenyl)ethenyl]-N,N-dimethylaniline

Produkt 1

HCID 54074224HCID 54074224, VerbindungAusbeute 80,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 72391,2-DichlorobenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

Into a mixture of 25 ml of acetic anhydride and 75 ml of o-dichlorobenzene, 13.4 g of 1-(p-ethoxyphenyl)-1-(p-dimethylaminophenyl)ethylene (melting at 110°-111° C.) and 21.5 g of tetrachlorophthalic anhydride were added and the mixture was stirred for 6 hours at 120° C. After adding the reaction mixture into 200 ml of water and making the mixture alkaline by sodium hydroxide, the alkaline mixture was extracted with 70 ml of toluene. The solid matter obtained by distilling off toluene from the extract was recrystallized from acetone while purifying with activated carbon to obtain 16.2 g of pale yellow crystals in a yield of 80.8%.

Aufarbeitung

  1. additionwere added
  2. extractionthe alkaline mixture was extracted with 70 ml of toluene
  3. customThe solid matter obtained
  4. distillationby distilling off toluene from the extract
  5. customwas recrystallized from acetone
  6. customwhile purifying with activated carbon

Quellen und Nachweise

ORD-Eintrag
ord-ec5b4c14384a4b7198296d0079296fdd
Quelldatensatz
uspto-grants-1989_05
Patentnummer
US04835291

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