反应详情

温度

0 °C

To a solution of ethyl 3-methoxy-5-methylphenylacetate (3.0 g; 14 mmol; from step (iv) above) and ethyl formate (1.9 g; 26 mmol) in ether (75 mL) was added Na (0.39 g; 17 mmol) in small lumps. The solution was cooled to 0° C. and EtOH (abs.; 0.24 mL) was then added. To the resulting slurry was added ether (100 mL), EtOH (5 mL) and water until the slurry was dissolved. The aqueous phase was collected, acidified to pH 2 (HCl/aq) and extracted with ether. The organic phase was washed with NaHCO3/aq, dried (Na2SO4), and evaporated to yield 2 g (59%) of the sub-title compound.

1. dissolutionwas dissolved
2. customThe aqueous phase was collected
3. extractionextracted with ether
4. washThe organic phase was washed with NaHCO3/aq
5. dry with materialdried (Na2SO4)
6. customevaporated