반응 #59075
ord-b877ca9cf4694fe29ed1e742856a09bc
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1농축The reaction mixture was then concentrated
- 2기타partitioned between ethyl acetate and water
- 3기타The organic layer was separated
- 4세척washed with water
- 5건조brine, dried over sodium sulfate
- 6농축concentrated
- 7기타to give orange solid
- 8기타Purification on silica gel with 20% methanol in methylene chloride
실험 절차
The mixture containing N-(4-(4-(methylamino)-3-nitrophenoxy)pyridin-2-yl)-2-chloroacetamide (1 eq), 1-ethylpiperazine (3 eq), and potassium carbonate (4 eq) was stirred in dimethylformamide at 60° C. for 1 hour. The reaction mixture was then concentrated and partitioned between ethyl acetate and water. The organic layer was separated and washed with water then brine, dried over sodium sulfate and concentrated to give orange solid. Purification on silica gel with 20% methanol in methylene chloride gave N-(4-(4-(methylamino)-3-nitrophenoxy)pyridin-2-yl)-2-(4-ethylpiperazin-1-yl)acetamide as a red solid. HPLC=3.26 min; MS: MH+=415.