Dimethyl Sulfoxide → HCID 14834673, 화합물

HRID 1638677노트

반응식

HRID 1638677 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([F:11])=[C:4]([F:12])[C:3]=1[CH3:13].[F-:14].[K+].CS(C)=O>C1C=CC=CC=1>[F:14][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([F:11])=[C:4]([F:12])[C:3]=1[CH3:13]

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 522689Potassium FluorideHCID 14834653HCID 14834653, 화합물

생성물 1

HCID 14834673HCID 14834673, 화합물수율 48.9%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To 2-chloro-5,6-difluoro-3-nitrotoluene (1.0 g) are added spray-dried potassium fluoride (1.4 g), anhydrous dimethylsulfoxide (10 ml) and benzene (10 ml), and the moisture is removed by azeotropic distillation together with benzene. Subsequently, the mixture is stirred at 170°-180° C. under argon stream for 3.5 hours. After cooling, the reaction mixture is poured into ice water and extracted with diethyl ether. The extract is washed with water, dried and then the solvent is distilled off. The residue is purified by silica gel column chromatography (solvent, n-hexane) to give 2,5,6-trifluoro-3-nitrotoluene (0.45 g).

후처리

  1. customthe moisture is removed by azeotropic distillation together with benzene
  2. temperatureAfter cooling
  3. additionthe reaction mixture is poured into ice water
  4. extractionextracted with diethyl ether
  5. washThe extract is washed with water
  6. customdried
  7. distillationthe solvent is distilled off
  8. customThe residue is purified by silica gel column chromatography (solvent, n-hexane)

출처 및 근거

ORD 기록
ord-f0accb1d4b3c4731b37ca84c9413591d
출처 데이터셋
uspto-grants-1989_11
특허 번호
US04880806

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