Nitric Acid → 5-Fluoro-4-methyl-2-nitrobenzoic acid

HRID 34590노트

반응식

HRID 34590 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[N+:12]([C:8]1[CH:9]=[C:10]([CH3:11])[C:2]([F:1])=[CH:3][C:4]=1[C:5]([OH:7])=[O:6])([O-:14])=[O:13]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 676873-Fluoro-p-toluic acid

생성물 1

HCID 136574495-Fluoro-4-methyl-2-nitrobenzoic acid

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

50 g of 3-fluoro-4-methyl-benzoic acid are initially introduced into 100 ml of concentrated sulphuric acid, and a mixture consisting of 26 g of 98% strength nitric acid and 40 g of concentrated sulphuric acid is added dropwise at 20°-25°, while cooling with ice. The mixture is subsequently stirred at room temperature for 1 hour. The batch is then poured onto ice-water and the crystals are filtered off with suction and washed thoroughly with water. After drying and recrystallization from toluene, 48 g (74.3% of theory) of 2-nitro-4-methyl-5-fluorobenzoic acid of melting point m.p.: 163°-5° C. are obtained.

후처리

  1. additionis added dropwise at 20°-25°
  2. temperaturewhile cooling with ice
  3. additionThe batch is then poured onto ice-water
  4. filtrationthe crystals are filtered off with suction
  5. washwashed thoroughly with water
  6. customAfter drying
  7. customrecrystallization from toluene, 48 g (74.3% of theory) of 2-nitro-4-methyl-5-fluorobenzoic acid
  8. customare obtained

출처 및 근거

ORD 기록
ord-91c996f281b642f18e876d4e94f66608
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762844

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