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Sulfuric Acid → HCID 10859468, Verbindung

HRID 487793
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 487793
[Br:1][C:2]1[CH:7]=[C:6]([S:8]([CH3:11])(=[O:10])=[O:9])[C:5]([CH3:12])=[CH:4][C:3]=1[CH3:13].S(=O)(=O)(O)O.[Cl:19]Cl>>[Cl:19][C:4]1[C:3]([CH3:13])=[C:2]([Br:1])[CH:7]=[C:6]([S:8]([CH3:11])(=[O:10])=[O:9])[C:5]=1[CH3:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 1118Sulfuric AcidHCID 24526ChlorineHCID 10945260Benzene, 1-bromo-2,4-dimethyl-5-(methylsulfonyl)-

Produkt 1

HCID 10859468HCID 10859468, Verbindung

Versuchsvorschrift

2.0 g of the crude 4-bromo-6-methylsulfonyl-m-xylene obtained in Example 1 was added to 8 ml of 20% fuming sulfuric acid. A chlorine gas was flown little by little while stirring at room temperature in a reactor provided with a dry ice trap at the upper part. After one hour, the reaction liquor was added to ice, and was extracted twice with 30 ml of EDC. The EDC solution was washed with 50 ml of water and then with 20 ml of a saturated aqueous solution of common salt, and was dried over anhydrous sodium sulfate, concentrated under reduced pressure and dried to a solid, thus obtaining 2.2 g of a crude product of the above-identified aimed compound (purity measured by gas chromatography: 81.6%). A part of the crude product was recrystallized from methanol to obtain the above-identified aimed compound.

Aufarbeitung

  1. customprovided with a dry ice trap at the upper part
  2. additionthe reaction liquor was added to ice
  3. extractionwas extracted twice with 30 ml of EDC
  4. washThe EDC solution was washed with 50 ml of water
  5. dry with materialwith 20 ml of a saturated aqueous solution of common salt, and was dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customdried to a solid
  8. customthus obtaining 2.2 g of a crude product of the above-identified aimed compound (purity measured by gas chromatography: 81.6%)
  9. customA part of the crude product was recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-3fd856981aac40f78a3bd619475bb9a4
Quelldatensatz
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05296634

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