반응 #1128826

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5-Fluoro-2-methyl-benzoxazole

Sulfuric acid

Sulfuric acid

Nitric acid

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5-Fluoro-2-methyl-6-nitro-benzoxazole

반응 조건

후처리

1. 1
   온도to maintain the temperature below 25° C
2. 2
   workup.ADDITIONAfter complete addition
3. 3
   workup.ADDITIONwas added dropwise
4. 4
   온도maintaining the temperature below 18° C
5. 5
   workup.ADDITIONAfter the addition
6. 6
   기타the cooling bath was removed
7. 7
   workup.ADDITIONwas poured onto 100 mL ice
8. 8
   workup.STIRRINGwith stirring
9. 9
   기타The solids were collected
10. 10
    세척washed with water (3×100 mL)
11. 11
    기타dried

실험 절차

5-Fluoro-2-methyl-benzoxazole (5.20 g, 0.0344 mol) was added to ice cooled Sulfuric acid (15.0 mL) such as to maintain the temperature below 25° C. After complete addition, a mixture of Sulfuric acid (2.75 mL) and Nitric acid (2.50 mL, 0.0536 mol) was added dropwise, maintaining the temperature below 18° C. After the addition was complete, the cooling bath was removed and the mixture was stirred at ambient temperature for 3 h, then was poured onto 100 mL ice with stirring. The solids were collected and washed with water (3×100 mL) and dried to give 5-Fluoro-2-methyl-6-nitro-benzoxazole as yellow solids. 1H-NMR (DMSO): 8.64 (d, 1H, J=5.4 Hz), 7.97 (d, 1H, J=10.8 Hz), 2.71 (s, 3H).

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