HRID975610

反应详情

EQUATION

反应方程式

HRID 975610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
96 °C

PROCEDURE

实验过程

A flask equipped with a magnetic stir bar and a water cooled condenser with an oil bubbler was charged with 1,2,4,5-tetrachlorobenzene (648 mg, 3.0 mmol), sodium tetrahydridoborate (1135 mg, 30.0 mmol), bis(η5 -cyclopentadienyl)titanium dichloride (75 mg, 0.3 mmol) and 1-methyl-2pyrrolidine (NMP; 30.0 ml). The reaction mixture was heated at 96° C. in an oil bath. After 4.25 hours, lithium chloride (1.09 g, 30.0 mmol) was added. Aliquots were withdrawn by syringe, quenched with water, and extracted with diethyl ether. The ether layer was analyzed with the results shown in the following table. Only trichlorobenzene was produced.

WORKUP

后处理

  1. customA flask equipped with a magnetic stir bar and a water cooled condenser with an oil bubbler
  2. customAliquots were withdrawn by syringe
  3. customquenched with water
  4. extractionextracted with diethyl ether