3,4,6-Trichloropyridazine → 3,6-Dichloro-4-methanesulfonylpyridazine
反応式
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1Cl.[Na+].[CH3:11][S:12]([O-:14])=[O:13]>O.C1COCC1.CN(C=O)C>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[S:12]([CH3:11])(=[O:14])=[O:13]参加物
4
実験手順
3,4,6-Trichloropyridazine (2.5 g; 13.6 mmol) and methanesulfinic acid sodium salt (2.78 g, 27.26 mmol) were stirred in 20 ml of a solvent mixture of water/THF/DMF (5:10:5) at RT for 30 h. The solvent was removed under reduced pressure and the residue was partitioned between ethyl acetate and saturated ammonium chloride solution. The organic phase was removed and concentrated, and the crude product was purified by flash chromatography (dichloromethane:methanol). Yield: 1.4 g
後処理
- customThe solvent was removed under reduced pressure
- customthe residue was partitioned between ethyl acetate and saturated ammonium chloride solution
- customThe organic phase was removed
- concentrationconcentrated
- customthe crude product was purified by flash chromatography (dichloromethane:methanol)
出典と根拠
- ORDレコード
- ord-f3c01bf9600a496c89aa13cb31eb9f0c
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08076336B2
反応ノート
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