HRID917372

反应详情

EQUATION

反应方程式

HRID 917372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To 5 ml of N,N-dimethylformamide were dissolved 0.39 g (2.0 mmol) of 6-butoxynicotinic acid, synthesized by a method in accordance with one used in Intermediate Production Example 1, and 0.40 g (2.0 mmol) of 4,4-difluoro-3-methyl-3-butenyl methanesulfonate, followed by the addition of 0.34 g (4.0 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 3 hours. The reaction liquid was then poured in water and extracted with diethyl ether. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:7) to obtain 0.45 g (yield: 75%) of 4,4-difluoro-3-methyl-3-butenyl 6-butoxynicotinate.

WORKUP

后处理

  1. customsynthesized by a method in accordance with one
  2. customThe reaction liquid
  3. extractionextracted with diethyl ether
  4. washThe organic layer was washed with water
  5. dry with materialby drying over anhydrous magnesium sulfate and concentration under reduced pressure
  6. customThe residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:7)