HRID1521801

反应详情

EQUATION

反应方程式

HRID 1521801 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1,1′-(naphtho[1,2-b]thiophene-2,7-diyl)bis(2,2-dibromoethanone) (10b) (180 g, 310 mmol) obtained as above was dissolved in 500 ml of THF and the solution was cooled to 0° C. A mixture of diethyl phosphite (80 ml, 620 mmol) and triethylamine (86 ml, 210 mmol) in 50 ml THF was added dropwise to the solution which was kept on an ice bath. After the addition, the ice bath was removed and the reaction mixture was stirred at room temperature for 2 hr. The volume of THF was reduced by rotary evaporation to obtain a solid residue which was washed with pentane to afford 1,1′-(naphtho[1,2-b]thiophene-2,7-diyl)bis(2-bromoethanone) as a brown solid (10c) (110 g, 84%).

WORKUP

后处理

  1. additionwas added dropwise to the solution which
  2. customwas kept on an ice bath
  3. additionAfter the addition
  4. customthe ice bath was removed
  5. customThe volume of THF was reduced by rotary evaporation
  6. customto obtain a solid residue which
  7. washwas washed with pentane