HRID648989

反应详情

EQUATION

反应方程式

HRID 648989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Stir slowly, an intimate mixture of 220 g of 2-bromo-4,6-dichlorotoluene, 167 g of N-bromosuccinimide and 1 g of benzoyl peroxide in a flask (equipped with a condenser and stirrer) immersed in an 145° C. oil bath. After 10-20 min a vigorous eruption occurs and the mixture liquifies. Remove the oil bath and stir for an additional 5 min. Add 1.5 L of CCl4 slowly through the condenser. Cool the mixture and suction filter the resulting reaction mixture. Wash the filtrate with 5% aqueous sodium thiosulfate, dry over anhydrous K2CO3, filter and evaporate to a residue. Fractionally distill the residue to give 134 g of 2-bromo-4,6-dichlorobenzyl bromide, bp 94°-97° C. (0.2 tor).

WORKUP

后处理

  1. custom(equipped with a condenser and stirrer)
  2. customimmersed in an 145° C.
  3. customRemove the oil bath
  4. stirringstir for an additional 5 min
  5. additionAdd 1.5 L of CCl4 slowly through the condenser
  6. temperatureCool the mixture and suction
  7. filtrationfilter
  8. customthe resulting reaction mixture
  9. washWash the filtrate with 5% aqueous sodium thiosulfate
  10. dry with materialdry over anhydrous K2CO3
  11. filtrationfilter
  12. customevaporate to a residue
  13. distillationFractionally distill the residue