반응 #60496

반응 방정식

nitric acid

4-bromo-1,2-dimethoxybenzene

→

title compound

1-Bromo-4,5-dimethoxy-2-nitrobenzene

용매

acetic acid

반응 조건

후처리

1. 1
   온도The reaction mixture was warmed to 15° C.
2. 2
   workup.STIRRINGstirring
3. 3
   온도The reaction mixture was cooled to 0° C.
4. 4
   workup.STIRRINGstirred
5. 5
   추출extraction
6. 6
   세척washed with water
7. 7
   건조After drying the organic layer over anhydrous magnesium sulfate
8. 8
   여과the desiccant was filtered off
9. 9
   농축the filtrate was concentrated under reduced pressure
10. 10
    기타The obtained crude product
11. 11
    기타was recrystallized from ethanol

실험 절차

A mixture of concentrated nitric acid (14 mL) and acetic acid (42 mL) was cooled to 10° C. while stirring, and then 4-bromo-1,2-dimethoxybenzene (2 g, 9.21 mmol) was gradually added to the stirred mixture. The reaction mixture was warmed to 15° C., and stirring was continued for 60 minutes. The reaction mixture was cooled to 0° C. and stirred while adding ice water, and then extraction was performed with ether. The obtained organic layer was neutralized with saturated aqueous solution of sodium hydrogencarbonate and potassium carbonate, and then washed with water. After drying the organic layer over anhydrous magnesium sulfate, the desiccant was filtered off and the filtrate was concentrated under reduced pressure. The obtained crude product was recrystallized from ethanol to give 2.09 g of the title compound as light yellow crystals.

출처