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Acetic Anhydride → HCID 57151183, Verbindung

HRID 2057719
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2057719
[Cl:1][C:2]1[C:12]2[C:13]3C(CC[C:8]=3[CH:9]=[CH:10][C:11]=2[Cl:14])=[CH:4][CH:3]=1.[C:15]([O:18][C:19](=[O:21])[CH3:20])(=[O:17])[CH3:16].[OH-].[K+].Cl[O-].[Na+]>O.O.O.O.C([O-])(=O)C.[Co+2].C([O-])(=O)C.O.O.O.O.C([O-])(=O)C.[Mn+2].C([O-])(=O)C.[Na+].[Br-].O.ClC1C=CC=CC=1.C(O)(=O)C>[Cl:1][C:2]1[C:12]2[C:13](=[CH:8][CH:9]=[CH:10][C:11]=2[Cl:14])[C:16]([C:15]([O:18][C:19]([C:20]2[C:13]3[C:12](=[C:11]([Cl:14])[CH:10]=[CH:9][CH:8]=3)[C:2]([Cl:1])=[CH:3][CH:4]=2)=[O:21])=[O:17])=[CH:4][CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 4

HCID 7918Acetic AnhydrideHCID 14797Potassium HydroxideHCID 1457305,6-Dichloro-1,2-dihydroacenaphthyleneHCID 23665760Sodium Hypochlorite

Produkt 1

HCID 57151183HCID 57151183, VerbindungAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 6

HCID 61372
Cobalt(II) acetate tetrahydrate
Katalysator
HCID 93021Manganese acetate tetrahydrateKatalysator
HCID 253881Sodium BromideKatalysator
HCID 176Acetic AcidLösungsmittel
HCID 962WaterLösungsmittel
HCID 7964ChlorobenzeneLösungsmittel2×

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

There was provided a 300 ml flask which was equipped with an agitator and a thermometer and provided with a gas feed port and a gas exhaust port attached with a condenser. The flask was charged with 22.3 g of 5,6-dichloroacenaphthene, 0.6 g of cobalt acetate tetrahydrate, 0.2 g of manganese acetate tetrahydrate, 0.2 g of NaBr, 10 ml of acetic acid, 90 ml of chlorobenzene, and 17 ml of acetic anhydride. The reaction system was heated to 65° C., into which air was blown for oxidation at a rate of 50 ml/min. The reaction was continued for 20 hours, during which the system was gradually heated up to 95° C. After completion of the reaction, the acetic acid was removed by distillation together with the chlorobenzene. To the remaining reaction mixture were added 50 ml of chlorobenzene and 400 ml of water dissolving therein 27 g of KOH, into which 32 ml of a sodium hypochlorite solution (13.6%) was dropped at 70°-100° C. The chlorobenzene was removed from the reaction solution, followed by treating with active carbon and filtering. The filtrate was treated with an acid to permit precipitation and the precipitate was filtered, washed with water and dried to obtain 23.5 g of 4,5-dichloronaphthalic anhydride. The yield was 88.0%.

Aufarbeitung

  1. customThere was provided a 300 ml flask which
  2. customwas equipped with an agitator
  3. customa thermometer and provided with a gas feed port
  4. customattached with a condenser
  5. temperaturethe system was gradually heated up to 95° C
  6. customAfter completion of the reaction
  7. customthe acetic acid was removed by distillation together with the chlorobenzene
  8. customTo the remaining reaction mixture
  9. customThe chlorobenzene was removed from the reaction solution
  10. additionby treating with active carbon
  11. filtrationfiltering
  12. additionThe filtrate was treated with an acid
  13. customprecipitation
  14. filtrationthe precipitate was filtered
  15. washwashed with water
  16. customdried

Quellen und Nachweise

ORD-Eintrag
ord-cd47e84624ac4461887805ce5a767c80
Quelldatensatz
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04212813

Notizen zur Reaktion

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