Nitric Acid → 5-Fluoro-2-methyl-6-nitro-1,3-benzoxazole

HRID 1041644

반응식

HRID 1041644 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([CH3:10])=[N:7][C:6]=2[CH:11]=1.S(=O)(=O)(O)O.[N+:17]([O-])([OH:19])=[O:18]>>[F:1][C:2]1[C:3]([N+:17]([O-:19])=[O:18])=[CH:4][C:5]2[O:9][C:8]([CH3:10])=[N:7][C:6]=2[CH:11]=1

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2회HCID 27693505-Fluoro-2-methylbenzoxazole

생성물 1

HCID 136277005-Fluoro-2-methyl-6-nitro-1,3-benzoxazole

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).

후처리

  1. temperatureto maintain the temperature below 25° C
  2. additionAfter complete addition
  3. additionwas added dropwise
  4. temperaturemaintaining the temperature below 18° C
  5. additionAfter the addition
  6. customthe cooling bath was removed
  7. additionwas poured onto 100 mL ice
  8. stirringwith stirring
  9. customThe solids were collected
  10. washwashed with water (3×100 mL)
  11. customdried

출처 및 근거

ORD 기록
ord-f3e0e7316dfb4103befc1133ecc94197
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552186B2

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