反应详情

温度

-78 °C

A solution of 1.5M methyllithium/ether (26 mL, 0.039 mol) was added dropwise to a solution of N-methyl-N-methoxy-2-chloro-5-sulfamoylthiophene-3-carboxamide (3.25 g, 0.011 mol) in dry THF (145 mL) under a nitrogen atmosphere, cooled to -78° C. After two hours, the reaction mixture was poured carefully into ice/dil. HCl and the product was extracted into ethyl acetate. This extract was washed with water and brine, dried (Na2SO4), filtered and evaporated to give 2.82 g of crude solid product. This material was chromatographed on silica gel and eluted with 40% ethyl acetate/hexane to give 1.7 g (74%) of product. Recrystallization from ethyl acetate/hexane gave 1.68 g of product, mp 128°-130° C.

1. additionthe reaction mixture was poured carefully into ice/dil
2. extractionHCl and the product was extracted into ethyl acetate
3. washThis extract was washed with water and brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated
7. customto give 2.82 g of crude solid product
8. customThis material was chromatographed on silica gel
9. washeluted with 40% ethyl acetate/hexane