Cesium carbonate → 3-(3-Nitrophenylthio)pyridine
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([SH:10])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].Br[C:12]1[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=1.O=C1CCCCC1C(OCC)=O.C(=O)([O-])[O-].[Cs+].[Cs+]>CS(C)=O.[Cu](I)I>[N+:1]([C:4]1[CH:5]=[C:6]([S:10][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=2)[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2]参加物
7
実験手順
3-nitrophenylmercaptan (5 g, 32 mmol), 3-bromopyridine (6.1 g, 38.6 mmol), ethyl 2-oxocyclohexylformate (1.1 g, 6.5 mmol), copper iodide (608 mg, 4.2 mmol), cesium carbonate (2.3 g, 70.6 mmol) were dissolved in 500 ml of DMSO, reacted under microwaves at 100° C. for 8 h. After being extracted with water and DCM, the organic phase was dried and separated with column chromatography to obtain an object product 3.2 g.
後処理
- customreacted under microwaves at 100° C. for 8 h
- extractionAfter being extracted with water and DCM
- customthe organic phase was dried
- customseparated with column chromatography
出典と根拠
- ORDレコード
- ord-a0d13f15a77e4ef9bae4bf6373c2ca64
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181244B1
反応ノート
読み込み中…
