HRID1074214

反应详情

EQUATION

反应方程式

HRID 1074214 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound 2',4'-difluoro-4(2-chloroethoxy)biphenyl is prepared by a process wherein to a solution of 15 g of sodium hydroxide in 30 ml of water there is added 68.2 g of 4-(2',4'-difluorophenyl)phenol and 106 g of 2-chloroethyl-p-toluene-sulfonate. The mixture is heated to about 95°-100° C. while stirring (at 96°-98° C. an exothermic reaction occurs) and maintained at this temperature for 5 hours. The resulting material is diluted with dichloromethane, washed with water, and evacuated until dry. The crude product is crystallized using isopropyl alcohol to yield 62 g (69% of theory) of the final product. If a further crop (9 g) of pure product can be obtained from the mother liquor, the total yield of the product is 80% of theory.

WORKUP

后处理

  1. temperatureThe mixture is heated to about 95°-100° C.
  2. customan exothermic reaction
  3. temperaturemaintained at this temperature for 5 hours
  4. washwashed with water
  5. customevacuated
  6. customuntil dry
  7. customThe crude product is crystallized