HRID615436

反应详情

EQUATION

反应方程式

HRID 615436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a stirred reaction vessel was placed 2.31 grams (0.010 mole) of 2-chloro-6-(trichloromethyl)pyridine, 20 ml of N-methylpyrrolidone and 1.35 grams (0.011 mole) of dimethylphosphite. The mixture was heated for about 21/2 hours. During this period, 50 percent aqueous sodium hydroxide was slowly added to maintain the pH slightly basic. At the end of the reaction period, there was 1% of the pyridine starting material remaining. Additionally, it was found that 0.0225 mole of the aqueous sodium hydroxide had been added. The reaction mixture was poured into water, extracted with methylene chloride, dried and the methylene chloride removed by evaporation, to yield 1.6 grams (80% of theoretical) of crude 2-chloro-6-(dichloromethyl)pyridine.

WORKUP

后处理

  1. customIn a stirred reaction vessel
  2. temperatureThe mixture was heated for about 21/2 hours
  3. waitDuring this period
  4. temperatureto maintain the pH slightly basic
  5. customAt the end of the reaction period, there
  6. additionhad been added
  7. extractionextracted with methylene chloride
  8. customdried
  9. customthe methylene chloride removed by evaporation