Reaktion #50893

Reaktionsgleichung

3-bromodibenzothiophene-5-oxide

sulfuric acid

nitric acid

→

3-bromo-7-nitrodibenzothiophene-5-oxide

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA flask equipped with a stirrer
2. 2
   Temperaturthe resulting mixture was cooled to −2° C
3. 3
   Sonstigeto terminate
4. 4
   Sonstigethe reaction
5. 5
   workup.STIRRINGstirred further
6. 6
   FiltrationThe reactant was filtered
7. 7
   Waschenwashed with water
8. 8
   Sonstigedried
9. 9
   SonstigeThe resulting dry cake
10. 10
    Waschenwas washed with ethanol

Vorschrift

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:

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