反应详情

3-tert-Butyl-N-methoxy-5-(2-methoxyethoxy)-N-methylbenzamide (O3.043; 1.35 g) was dissolved in THF (40 ml), methylmagnesium bromide (3.05 ml, 3 M in ether) was added dropwise at 0° C. and then the mixture was stirred at RT for 2 h. Then the mixture was admixed with 1 N hydrochloric acid (50 ml), diluted with water and extracted by shaking three times with EA. Then the combined EA phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (40 g cartridge, n-heptane/EA gradient of 0-30% in 30 min). 1.0 g of the title compound were obtained.

1. extractionextracted
2. stirringby shaking three times with EA
3. dry with materialThen the combined EA phases were dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified
7. customsilica gel (40 g cartridge, n-heptane/EA gradient of 0-30% in 30 min)