Реакция #2173713

Уравнение реакции

2-(ethylphenylamino)ethyl acetate

sodium acetate

phosphoryl chloride

→

2-(ethyl(4-formylphenyl)amino)ethyl acetate

Растворители

dimethylformamide

dimethylformamide

Условия реакции

Обработка

1. 1
   workup.STIRRINGthis mixture was stirred for 5 hours at 40° C
2. 2
   ЭкстракцияAn organic layer was extracted with ethyl acetate
3. 3
   Промывкаwashed with water
4. 4
   Сушкаdried over sodium sulfate
5. 5
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
6. 6
   Другоеthe resulting coarse product was purified by silica gel column chromatography

Методика

To 16.1 g of dimethylformamide was dropwise added 33.7 g of phosphoryl chloride while stirring under ice cooling. Further, 30 ml of a solution of 41.5 g of 2-(ethylphenylamino)ethyl acetate in dimethylformamide was added dropwise, and this mixture was stirred for 5 hours at 40° C. This reaction solution was poured into 1,000 ml of sodium acetate aqueous solution. An organic layer was extracted with ethyl acetate, washed with water, and then dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the resulting coarse product was purified by silica gel column chromatography to obtain 35.3 g of 2-(ethyl(4-formylphenyl)amino)ethyl acetate.

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