反応 #2689

反応方程式

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

Potassium carbonate

methyl iodide

→

pure product

収率 88.3%

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

収率 88.3%

溶媒

DMF

反応条件

後処理

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

実験手順

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.

出典