四氧化硫 → 2-Methyl-3,4,6-trifluorobenzonitrile

HRID 1272

反应方程式

HRID 1272 反应方程式
[CH3:1][C:2]1[C:8]([F:9])=[C:7]([F:10])[CH:6]=[C:5]([F:11])[C:3]=1N.S(=O)(=O)(O)O.N([O-])=O.[Na+].[C-:21]#[N:22].[K+].[OH-].[NH4+]>S([O-])([O-])(=O)=O.[Cu+2].O>[CH3:1][C:2]1[C:8]([F:9])=[C:7]([F:10])[CH:6]=[C:5]([F:11])[C:3]=1[C:21]#[N:22]

参与物

8

反应物 5

HCID 1118四氧化硫HCID 9032氰化钾HCID 14923氨水HCID 226251783,4,6-Trifluoro-2-methylanilineHCID 23668193亚硝酸钠

产物 1

HCID 226251752-Methyl-3,4,6-trifluorobenzonitrile收率 38.2%

试剂、催化剂与溶剂 2

HCID 24462HCC38 CELLS|人乳腺导管癌贴壁细胞催化剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

实验过程

To 2-methyl-3,4,6-trifluoroaniline (10.6 g) is added a mixture of conc. sulfuric acid (13.8 ml) and water (46 ml) and the mixture is cooled. Thereto an aqueous solution (20 ml) of sodium nitrite (5.5 g) is added dropwise at 0°-5° C. The solution is gradually added to a mixture of copper (II) sulfate 5 hydrate (41 g), potassium cyanide (43 g), ammonium hydroxide (60 ml) and water (260 ml) at 10°-30° C. The mixture is extracted with dichloromethane and the extract is dried over sodium sulfate, concentrated and the residue is purified with column chromatography (silica-gel, dichloromethane:n-hexane=1:4) to give 2-methyl-3,4,6-trifluorobenzonitrile (4.3 g).

后处理

  1. temperaturethe mixture is cooled
  2. extractionThe mixture is extracted with dichloromethane
  3. dry with materialthe extract is dried over sodium sulfate
  4. concentrationconcentrated
  5. customthe residue is purified with column chromatography (silica-gel, dichloromethane:n-hexane=1:4)

来源与证据

ORD记录
ord-1e9ca78c8b7943d3b81ed784f0fbf2a2
来源数据集
uspto-grants-1998_03
专利号
US05723648

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