Nitric Acid → 6-fluoro-5-nitro-2(3H)-benzoxazolone

HRID 414635노트

반응식

HRID 414635 반응식
[F:1][C:2]1[CH:11]=[CH:10][C:5]2[NH:6][C:7](=[O:9])[O:8][C:4]=2[CH:3]=1.[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[F:1][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]2[NH:6][C:7](=[O:9])[O:8][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 144573586-Fluoro-1,3-benzoxazol-2(3H)-one

생성물 1

HCID 137721116-fluoro-5-nitro-2(3H)-benzoxazolone수율 85%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A solution cf 6-fluoro-2(3H)-benzoxazolone (1.0 g) in 80% aqueous sulfuric acid (6.5 g) was cooled to 0° to 5° C., and 60% nitric acid (0.8 g) was gradually added thereto at 0° to 5° C. The resultant mixture was stirred at the same temperature for 30 minutes and poured onto ice water. The precipitated crystals were collected by filtration, washed with water and dried to give 6-fluoro-5-nitro-2(3H)-benzoxazolone (1.1 g). m.p., 175.4° C. 1H-NMR (CDCl3 +DMSO-D6) δ ppm: 4.0 (1H, broad), 6.8-7.9 (3H, m).

후처리

  1. customat 0° to 5° C
  2. additionpoured onto ice water
  3. filtrationThe precipitated crystals were collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-399878f95d164f8ea6458e46497d883e
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04792605

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