聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 3,4-Dichloro-5-fluoro-2-picoline

HRID 1859

反应方程式

HRID 1859 反应方程式
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][N:5]=[C:4]([CH3:9])[CH:3]=1.C(O[Cl:15])(C)(C)C.O>C(Cl)(Cl)Cl>[Cl:15][C:3]1[C:4]([CH3:9])=[N:5][CH:6]=[C:7]([F:8])[C:2]=1[Cl:1]

参与物

5

反应物 3

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 521297次氯酸叔丁酯HCID 196914104-氯-5-氟-2-甲基吡啶2 次

产物 1

HCID 196912453,4-Dichloro-5-fluoro-2-picoline

试剂、催化剂与溶剂 1

HCID 6212三氯甲烷溶剂

反应条件

温度
0 °C

实验过程

To 0.87 g (6 mmol) of 4-chloro-5-fluoro-2-picoline, the product of Example 66, in 20 mL of chloroform cooled to -45° C., is added 0.75 mL of t-butylhypochlorite. The reaction mixture is stirred at -45° C. for 2 hours and at 0° C. for 2 hours. The reaction mixture is then poured into water and the resultant aqueous mixture is extracted with methylene chloride. The organic solution is dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure and distilled to afford the title compound.

后处理

  1. extractionthe resultant aqueous mixture is extracted with methylene chloride
  2. dry with materialThe organic solution is dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. distillationdistilled

来源与证据

ORD记录
ord-1ecb12c0a720485081b2a903dedaad68
来源数据集
uspto-grants-1998_03
专利号
US05726182

关联笔记

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