Potassium Nitrate → Benzoic acid,2,3,6-trifluoro-5-nitro-

HRID 1638663

반응식

HRID 1638663 반응식
[F:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[C:7]([F:12])[C:3]=1[C:4]([OH:6])=[O:5].[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[F:12][C:7]1[C:8]([N+:13]([O-:15])=[O:14])=[CH:9][C:10]([F:11])=[C:2]([F:1])[C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

4

반응물 2

HCID 24434Potassium NitrateHCID 5200622,3,6-Trifluorobenzoic acid

생성물 1

HCID 15631828Benzoic acid,2,3,6-trifluoro-5-nitro-수율 83.4%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

2,3,6-Trifluorobenzoic acid (21.0 g) is added to conc. sulfuric acid (120 ml) under ice-cooling. To the mixture is added dropwise a solution of potassium nitrate (14.5 g) in conc sulfuric acid (30 ml) at below 20° C. After the addition, the mixture is stirred at room temperature for one hour. The reaction mixture is poured into ice water and extracted with diethyl ether. The extract is dried over magnesium sulfate, and then the solvent is distilled off. The residue is recrystallized from dichloromethane-n-hexane to give 2,5,6-trifluoro-3-nitrobenzoic acid (22 g), as colorless prisms, m.p. 98°-99° C.

후처리

  1. temperaturecooling
  2. additionAfter the addition
  3. extractionextracted with diethyl ether
  4. dry with materialThe extract is dried over magnesium sulfate
  5. distillationthe solvent is distilled off
  6. customThe residue is recrystallized from dichloromethane-n-hexane

출처 및 근거

ORD 기록
ord-b5254972de5341e0b25ff1d9a8773f6d
출처 데이터셋
uspto-grants-1989_11
특허 번호
US04880806

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