반응 #73969
ord-199563e105234712aa9009e8a9abcee2
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1추출the reaction mixture was extracted with DCM (2×25 mL)
- 2세척The combined orgaic layers were washed with water (10 mL), brine (10 mL)
- 3건조dried (Na2SO4)
- 4농축concentrated
- 5기타The crude material was purified by flash chromatography on silica gel eluting with 50% EtOAc in DCM
실험 절차
To a solution of (E)-ethyl 3-(4-(4-(chlorosulfonyl)phenoxy)-3,5-difluorophenyl)-2-methylacrylate (intermediate 41.3) (250 mg, 0.60 mmol) in DCM (3 mL) was added a solution of 2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethanamine (157 mg, 0.72 mmol) and triethylamine (72 mg, 0.72 mmol) in DCM (2 mL). After 15 minutes, water (10 mL) was added and the reaction mixture was extracted with DCM (2×25 mL). The combined orgaic layers were washed with water (10 mL), brine (10 mL), dried (Na2SO4) and concentrated. The crude material was purified by flash chromatography on silica gel eluting with 50% EtOAc in DCM to give the title compound (169 mg).