تفاعل #50893

ord-91ba5b85156544099c3e46dc24f4ee38

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA flask equipped with a stirrer
  2. 2
    درجة الحرارةthe resulting mixture was cooled to −2° C
  3. 3
    أخرىto terminate
  4. 4
    أخرىthe reaction
  5. 5
    workup.STIRRINGstirred further
  6. 6
    ترشيحThe reactant was filtered
  7. 7
    غسيلwashed with water
  8. 8
    أخرىdried
  9. 9
    أخرىThe resulting dry cake
  10. 10
    غسيلwas washed with ethanol

الإجراء التجريبي

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:

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06849202B2uspto-grants-2005_02