反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customA round-bottomed flask having
- customa volume of 50 mL and equipped with a glass stopper
- customa three-way cock was dried
- additioneach added
- customat intervals of 10 minutes
- temperatureNext, the temperature was slowly increased to room temperature
- temperatureThereafter, the solution was cooled to 0° C. again
- additionwas gradually added
- washThereafter, an organic layer was washed with 10 mL of an aqueous NaOH solution
- dry with materialdried with 50 g of sodium sulfate
- filtrationsubjected to dehydration and filtration steps