反应 #2689

反应方程式

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

Potassium carbonate

methyl iodide

→

pure product

收率 88.3%

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

收率 88.3%

溶剂

DMF

反应条件

后处理

1. 1
   温度After cooling to ambient temperature
2. 2
   过滤The precipitate was filtered off
3. 3
   其他the solution was evaporated
4. 4
   workup.DISSOLUTIONThe residue was dissolved in saturated aqueous NaHCO3
5. 5
   干燥the organic phase was dried (Na2SO4)
6. 6
   过滤filtered
7. 7
   其他evaporated

实验过程

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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