Sodium Chloride → 1-(Pyridazin-4-yl)ethan-1-one
反応式
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]=1参加物
5
実験手順
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).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-b192313b8b12471b9e30334c74e0da97
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08440666B2
反応ノート
読み込み中…