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Nitric Acid → 3-Bromo-7-nitrodibenzothiophene-5-oxide

HRID 22615
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 22615
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=3[S:7](=[O:14])[C:6]=2[CH:15]=1.S(=O)(=O)(O)O.[N+:21]([O-])([OH:23])=[O:22]>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:9]3[CH:10]=[CH:11][C:12]([N+:21]([O-:23])=[O:22])=[CH:13][C:8]=3[S:7](=[O:14])[C:6]=2[CH:15]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 218951323-Bromodibenzothiophene-5-oxide

Produkt 1

HCID 218950963-Bromo-7-nitrodibenzothiophene-5-oxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

A flask equipped with a stirrer and a thermometer was charged with 69.8 g of glacial acetic acid and 27.9 g of 3-bromodibenzothiophene-5-oxide prepared in Example 1-1 in a nitrogen atmosphere, and cooled to 10° C. 239.8 g of concentrated sulfuric acid was added dropwise, and the resulting mixture was cooled to −2° C. Then 72.0 g of 70 wt % nitric acid was added dropwise at −2 to 8° C., and the resulting mixture was stirred at or below 5° C. for 2 hours. The reaction mass was poured into 1200 g of ice water to terminate the reaction, and stirred further. The reactant was filtered, washed with water, and dried. The resulting dry cake was washed with ethanol to obtain 31.9 g of 3-bromo-7-nitrodibenzothiophene-5-oxide. The product was subjected to elemental analysis, the results of which are as follows:

Aufarbeitung

  1. customA flask equipped with a stirrer
  2. temperaturethe resulting mixture was cooled to −2° C
  3. customto terminate
  4. customthe reaction
  5. stirringstirred further
  6. filtrationThe reactant was filtered
  7. washwashed with water
  8. customdried
  9. customThe resulting dry cake
  10. washwas washed with ethanol

Quellen und Nachweise

ORD-Eintrag
ord-91ba5b85156544099c3e46dc24f4ee38
Quelldatensatz
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06849202B2

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