Ethyl oxoacetate → Ethyl 2-((tert-butylsulfinyl)imino)acetate
反応式
O=[CH:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH3:8][C:9]([S:12]([NH2:14])=[O:13])([CH3:11])[CH3:10]>C(Cl)Cl>[C:9]([S:12]([N:14]=[CH:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:13])([CH3:11])([CH3:10])[CH3:8]参加物
4
実験手順
A mixture of ethyl 2-oxoacetate (50% solution in toluene; 4.066 g; 20.00 mmol), 2-methylpropane-2-sulfinamide (2.424 g; 20.00 mmol), and 4 angstrom molecular sieves (60 g) in anh. DCM (250 ml) was stirred at rt, under nitrogen, for 65 h. The reaction mixture was then filtered over celite, and the separated solids were washed with AcOEt (3×200 ml). The filtrate was then dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure affording ethyl 2-((tert-butylsulfinyl)imino)acetate as a yellow oil.
後処理
- filtrationThe reaction mixture was then filtered over celite
- washthe separated solids were washed with AcOEt (3×200 ml)
- dry with materialThe filtrate was then dried over anh. MgSO4
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
出典と根拠
- ORDレコード
- ord-b9eaeb5e5f914fa5b1bf67f151028b12
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09242970B2
反応ノート
読み込み中…