Реакция #2689

Уравнение реакции

2,2,6,6-Tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole-4-carboxylic acid

Potassium carbonate

methyl iodide

→

pure product

Выход 88.3%

2,2,6,6-Tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole-4-carboxylic acid methyl ester

Выход 88.3%

Растворители

DMF

Условия реакции

Обработка

1. 1
   ТемператураAfter cooling to ambient temperature
2. 2
   ФильтрацияThe precipitate was filtered off
3. 3
   Другоеthe solution was evaporated
4. 4
   workup.DISSOLUTIONThe residue was dissolved in saturated aqueous NaHCO3
5. 5
   Сушкаthe organic phase was dried (Na2SO4)
6. 6
   Фильтрацияfiltered
7. 7
   Другоеevaporated

Методика

2,2,6,6-Tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole-4-carboxylic acid (10.0 g, 38.0 mmol) was dissolved in dry DMF (100 mL). Potassium carbonate (15.2 g, 110.0 mmol) was added and the reaction was heated to 55° C. for 30 min. After cooling to ambient temperature, methyl iodide (15.6 g, 110.0 mmol) was added and the solution was stirred overnight. The precipitate was filtered off and the solution was evaporated. The residue was dissolved in saturated aqueous NaHCO3 and ether. The aqueous layer was discarded and the organic phase was dried (Na2SO4), filtered and evaporated to give 9.4 g (88%) of the pure product.

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