HRID29116
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
- -2.5 °C
PROCEDURE
实验过程
To dimethylformamide (1802 ml) that had been cooled to −10° C. was added sodium tert-butoxide (528.6 g) and the solution was stirred at −5 to 0° C. for 30 min. Triethyl 2-phosphonopropionate (1310 g) was added dropwise thereto at 10° C. or below. The solution was stirred at 2 to 5° C. for 1 hr, and 4-methylbenzaldehyde (600.8 g) was added dropwise thereto at 10° C. or below and the solution was stirred at room temperature for 1 hr. Water was added thereto and the solution was extracted with toluene. The extract was washed with water and the solvent was distilled off to give the title compound as an oil (1009 g, yield 98.8%).
WORKUP
后处理
- customat 10° C. or below
- stirringThe solution was stirred at 2 to 5° C. for 1 hr
- stirringat 10° C. or below and the solution was stirred at room temperature for 1 hr
- extractionthe solution was extracted with toluene
- washThe extract was washed with water
- distillationthe solvent was distilled off