반응 #57394

반응 방정식

4-methylbenzaldehyde

dimethylformamide

sodium tert-butoxide

Triethyl 2-phosphonopropionate

→

title compound

수율 98.8%

ethyl 2-methyl-3-(4-methylphenyl)-2-propenoate

수율 98.8%

용매

Water

반응 조건

후처리

1. 1
   기타at 10° C. or below
2. 2
   workup.STIRRINGThe solution was stirred at 2 to 5° C. for 1 hr
3. 3
   workup.STIRRINGat 10° C. or below and the solution was stirred at room temperature for 1 hr
4. 4
   추출the solution was extracted with toluene
5. 5
   세척The extract was washed with water
6. 6
   workup.DISTILLATIONthe solvent was distilled off

실험 절차

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%).

출처