Реакция #428831

Уравнение реакции

2-(1,1-dimethylprop-2-ynyloxy)propionic acid methyl ester

sulfuric acid

→

2-(1,1-dimethyl-2-oxopropoxy)propionic acid methyl ester

Выход 141.7%

Растворители

water

Условия реакции

Обработка

1. 1
   ТемператураThe reaction mixture is maintained at 60° C. for 8 hours
2. 2
   Температураcooled to ambient temperature
3. 3
   ЭкстракцияThe aqueous phase is extracted with diethyl ether (3×250 ml)
4. 4
   Промывкаwashed with water
5. 5
   Сушкаdried over anhydrous sodium sulfate
6. 6
   ФильтрацияThe mixture is filtered
7. 7
   Другоеthe filtrate is evaporated under reduced pressure
8. 8
   ДругоеThe residue is purified by column chromatography on silica gel

Методика

A mixture of mercury (II) acetate (7.76 g, 0.024 mol), sulfuric acid (9 ml, 0.09 mol) and water (450 ml) is heated at 60° C. 2-(1,1-dimethylprop-2-ynyloxy)propionic acid methyl ester (90 g, 0.529 mol) is added carefully at 60° C. The reaction mixture is maintained at 60° C. for 8 hours and cooled to ambient temperature. The aqueous phase is extracted with diethyl ether (3×250 ml), the organic phases are combined, washed with water, and dried over anhydrous sodium sulfate. The mixture is filtered, and the filtrate is evaporated under reduced pressure. The residue is purified by column chromatography on silica gel to give 2-(1,1-dimethyl-2-oxopropoxy)propionic acid methyl ester (24 g) as a colorless oil.

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