HRID70818

反应详情

EQUATION

反应方程式

HRID 70818 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

A round-bottomed flask having a volume of 50 mL and equipped with a glass stopper and a three-way cock was dried, and 890 mg (3.51 mmol) of 2-(2-chloronaphthalen-1-yl)-3-methylpyridine and 20 mL of dichloromethane were introduced thereinto. This colorless solution was cooled to 0° C., and then 1.59 g (69-75%) of m-CPBA (meta-chloroperbenzoic acid) was each added thereto three times at intervals of 10 minutes. Next, the temperature was slowly increased to room temperature, and the colorless solution was stirred for 2 hours. Thereafter, the solution was cooled to 0° C. again, and 10 mL of an aqueous NaOH solution having a concentration of 1M was gradually added. Thereafter, an organic layer was washed with 10 mL of an aqueous NaOH solution having a concentration of 1M and 10 mL of salt water, then dried with 50 g of sodium sulfate, and subjected to dehydration and filtration steps, thereby obtaining 947 mg of yellow oily 2-(2-chloronaphthalen-1-yl)-5-methylpyridine-1-oxide.

WORKUP

后处理

  1. customA round-bottomed flask having
  2. customa volume of 50 mL and equipped with a glass stopper
  3. customa three-way cock was dried
  4. additioneach added
  5. customat intervals of 10 minutes
  6. temperatureNext, the temperature was slowly increased to room temperature
  7. temperatureThereafter, the solution was cooled to 0° C. again
  8. additionwas gradually added
  9. washThereafter, an organic layer was washed with 10 mL of an aqueous NaOH solution
  10. dry with materialdried with 50 g of sodium sulfate
  11. filtrationsubjected to dehydration and filtration steps