Phosphorus oxychloride → 184913-07-3
反応式
[CH3:1][C:2]1[NH:7][C:6](=O)[C:5]2[CH:9]=[CH:10][S:11][C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[C:5]2[CH:9]=[CH:10][S:11][C:4]=2[CH:3]=[C:2]([CH3:1])[N:7]=1参加物
3
実験手順
A solution of 6.2 g of 6-methylthieno[3,2-c]pyridin-4(5H)-one in 30 ml of phosphoryl chloride was heated under reflux for 1 hour. After being cooled, the excess phosphoryl chloride was removed under reduced pressure, and the residue was poured into ice water, made basic with aqueous 2N sodium hydroxide and extracted with chloroform. The extract was washed successively with water and saturated saline, and dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the solvent was removed under reduced pressure to give 7.0 g of 4-chloro-6-methylthieno[3,2-c]pyridine as a brown oily material.
後処理
- temperatureunder reflux for 1 hour
- temperatureAfter being cooled
- customthe excess phosphoryl chloride was removed under reduced pressure
- additionthe residue was poured into ice water
- extractionextracted with chloroform
- washThe extract was washed successively with water and saturated saline
- dry with materialdried over anhydrous magnesium sulfate
- customThe drying agent was removed by filtration
- customthe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-866ebecf69084fe49ad3c55eb0b0c19f
- 出典データセット
- uspto-grants-2000_02
- 特許番号
- US06020342
反応ノート
読み込み中…