Sodium Chloride → 1-(Pyridazin-4-yl)ethan-1-one
반응식
CON(C)[C:4]([C:6]1[CH:11]=[CH:10][N:9]=[N:8][CH:7]=1)=[O:5].[CH3:13][Mg]Br.[Cl-].[Na+]>O1CCCC1>[N:9]1[CH:10]=[CH:11][C:6]([C:4](=[O:5])[CH3:13])=[CH:7][N:8]=1참가 물질
5
실험 절차
To N-methoxy-N-methylpyridazine-4-carboxamide (1.13 g, 6.76 mmol) in tetrahydrofuran (22 mL), methylmagnesium bromide (10.1 mL, 10.1 mmol, 1M in diethyl ether) was added dropwise at 0° C. in a nitrogen stream, and the resulting solution was stirred for 1 hour. After completion of the reaction, the reaction solution was mixed with saturated aqueous sodium chloride and extracted with chloroform, and the extract was dried over anhydrous sodium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/2→0/1) to give the desired product (42% yield).
후처리
- customAfter completion of the reaction
- extractionextracted with chloroform
- dry with materialthe extract was dried over anhydrous sodium sulfate
- customevaporated under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/2→0/1)
출처 및 근거
- ORD 기록
- ord-b192313b8b12471b9e30334c74e0da97
- 출처 데이터셋
- uspto-grants-2013_05
- 특허 번호
- US08440666B2
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