تفاعل #2689

معادلة التفاعل

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

Potassium carbonate

methyl iodide

→

pure product

المردود 88.3%

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

المردود 88.3%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling to ambient temperature
2. 2
   ترشيحThe precipitate was filtered off
3. 3
   أخرىthe solution was evaporated
4. 4
   workup.DISSOLUTIONThe residue was dissolved in saturated aqueous NaHCO3
5. 5
   تجفيفthe organic phase was dried (Na2SO4)
6. 6
   ترشيحfiltered
7. 7
   أخرىevaporated

الإجراء التجريبي

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.

المصدر