Dimethyl Sulfoxide → HCID 14834673、化合物

HRID 2351906ノート

反応式

HRID 2351906 の反応式
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]

参加物

5

反応物 3

HCID 679Dimethyl SulfoxideHCID 522689Potassium FluorideHCID 14834653HCID 14834653、化合物

生成物 1

HCID 14834673HCID 14834673、化合物収率 48.9%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-b2a9e171b4ec48629cd3d58742e1dd33
出典データセット
uspto-grants-1989_10
特許番号
US04874764

反応ノート

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