反应详情

To a solution of 5.67 g (20 mmol) of 36 in 75 mL of acetic acid was added a solution of 3.5 g of anhydrous sodium acetate (42.7 mmol) in 100 mL of acetic acid. This mixture was refluxed with stirring for 2 h. Solids were removed by filtration and washed with acetic acid. The filtrate was evaporated to approximately 30 mL, then poured into water and extracted with ether. The organic phase was washed with aqueous sodium carbonate, water, and brine. After drying over sodium sulfate, the solution was filtered and evaporated to give 5.69 g (86%) of 2-[(acetyloxy)methyl]-4-(2-chloroethoxy)-5-methoxybenzyl acetate (37) as a white solid, mp 79-80° C.

1. temperatureThis mixture was refluxed
2. customSolids were removed by filtration
3. washwashed with acetic acid
4. customThe filtrate was evaporated to approximately 30 mL
5. additionpoured into water
6. extractionextracted with ether
7. washThe organic phase was washed with aqueous sodium carbonate, water, and brine
8. dry with materialAfter drying over sodium sulfate
9. filtrationthe solution was filtered
10. customevaporated