Thionyl Chloride → 6,7-Dibromo-8-nitro-1,4-benzodioxane-5-carbonyl chloride

HRID 127433Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 127433
[Br:1][C:2]1[C:11]([Br:12])=[C:10]([N+:13]([O-:15])=[O:14])[C:5]2[O:6][CH2:7][CH2:8][O:9][C:4]=2[C:3]=1[C:16]([OH:18])=O.S(Cl)([Cl:21])=O>>[Br:1][C:2]1[C:11]([Br:12])=[C:10]([N+:13]([O-:15])=[O:14])[C:5]2[O:6][CH2:7][CH2:8][O:9][C:4]=2[C:3]=1[C:16]([Cl:21])=[O:18]

Komponenten

3

Edukt 2

HCID 24386Thionyl ChlorideHCID 205447596,7-Dibromo-8-nitro-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acid

Produkt 1

HCID 205447556,7-Dibromo-8-nitro-1,4-benzodioxane-5-carbonyl chlorideAusbeute 91 %

Versuchsvorschrift

96 g of 6,7-dibromo-8-nitro-1,4-benzodioxane-5-carboxylic acid and 200 ml of thionyl chloride were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was heated under reflux and then the excess thionyl chloride was removed under vacuum. The residue was dissolved in 100 ml of isopropyl ether and then the solvent removed and the produced air-dried. 91 g of 6,7-dibromo-8-nitro-1,4-benzodioxane-5-carbonyl chloride were obtained (M.P.: 215° C.; yield: 91%).

Aufarbeitung

  1. customprovided with an agitator
  2. temperatureThe mixture was heated
  3. temperatureunder reflux
  4. customthe excess thionyl chloride was removed under vacuum
  5. dissolutionThe residue was dissolved in 100 ml of isopropyl ether
  6. customthe solvent removed
  7. customthe produced air-dried

Quellen und Nachweise

ORD-Eintrag
ord-54a9003f37024b16a14b58440727f723
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255580

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