反应详情

A solution of 4-(4-(methylamino)-3-nitrophenoxy)pyridin-2-amine (1 eq) and triethylamine (2 eq) in tetrahydrofuran was treated with 2-chloroacetyl chloride and stirred for 15 minutes at room temperature. The reaction mixture was then concentrated and partitioned between ethyl acetate and water. The organic layer was separated and washed with brine, dried over sodium sulfate and concentrated in vacuum to give crude product. Purification on silica gel with 2% methanol in methylene chloride gave N-(4-(4-(methylamino)-3-nitrophenoxy)pyridin-2-yl)-2-chloroacetamide as a bright orange solid. HPLC=3.82 min; MS: MH+=337.

1. concentrationThe reaction mixture was then concentrated
2. custompartitioned between ethyl acetate and water
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuum
7. customto give crude product
8. customPurification on silica gel with 2% methanol in methylene chloride