反应详情

N-Methoxy-N-methyl-3-morpholin-4-yl-5-(pentafluorosulfanyl)benzamide (2.38 g) was dissolved in THF (50 ml), methylmagnesium bromide (4.22 ml, 3 M in ether) was added dropwise at 0° C. and then the mixture was stirred at RT for 2 h. Then 1N hydrochloric acid (100 ml) was added, and the mixture was diluted with water and extracted by shaking three times with EA. Thereafter, the combined EA phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (80 g cartridge, n-heptane/EA gradient of 0-70% within 40 min). 1.1 g of the title compound were obtained.

1. extractionextracted
2. stirringby shaking three times with EA
3. dry with materialThereafter, the combined EA phases were dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified
7. customsilica gel (80 g cartridge, n-heptane/EA gradient of 0-70% within 40 min)