HRID463452

反应详情

EQUATION

反应方程式

HRID 463452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

A mixture of 100 ml dimethylformamide (DMF), 75 g (0.035 mole) 4-amino-2,5-dichlorophenol, hydrochloride, and 3.0 g (0.05 mole) KOH (pellets ground to powder) was placed in a 500 ml 3-necked round bottom flask fitted with a mechanical stirrer, thermometer and reflux condenser and was stirred for about 1 hour. It was then heated to 85° C. with stirring and 6.0 g (0.06 mole) of tetrafluoroethylene was bubbled in while heating at 85°-90° C. The addition took about 10 minutes. The reactor and contents were cooled in an ice water bath and 200 ml of water were added. The product was extracted with 200 ml methylene chloride and then again with 100 ml methylene chloride. The extracts were combined and the solvents removed by vacuum distillation. A residue (7 g) remained.

WORKUP

后处理

  1. customwas placed in a 500 ml 3-necked round bottom flask
  2. customfitted with a mechanical stirrer
  3. temperaturethermometer and reflux condenser
  4. stirringwith stirring
  5. temperaturewhile heating at 85°-90° C
  6. additionThe addition
  7. waittook about 10 minutes
  8. temperatureThe reactor and contents were cooled in an ice water bath
  9. extractionThe product was extracted with 200 ml methylene chloride
  10. customthe solvents removed by vacuum distillation