HRID232719

反应详情

EQUATION

反应方程式

HRID 232719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 4,5-dichloro-2-(3,4-dichlorophenyl)-pyrrole-3-carbonitrile (5.0 g, 0.016 mol) dissolved in 300 mL of tetrahydrofuran is added, portionwise, potassium t-butoxide (2.75 g, 0.025 mol) with ice cooling and stirring. The cooled mixture is treated with a solution of 1-chloroethyl ethyl ether (2.31 g, 0.021 mol) in 15 mL of tetrahydrofuran at 10° C. over a 5 minute period. The mixture is stirred for 1/2 hour at ambient temperatures, evaporated to a volume of 50 mL and poured into a mixture of 200 mL of ethyl acetate and 100 mL of water. The organic layer is separated, washed with water (2×100 mL), saturated NaCl solution (1×100 mL), dried over anhydrous magnesium sulfate and evaporated to give the title product 5.9 g, mp 124°-126° C.

WORKUP

后处理

  1. additionis added
  2. customevaporated to a volume of 50 mL
  3. additionpoured into a mixture of 200 mL of ethyl acetate and 100 mL of water
  4. customThe organic layer is separated
  5. washwashed with water (2×100 mL), saturated NaCl solution (1×100 mL)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated