Sodium Hydroxide → 1-Chloro-5,7-dimethoxyphthalazine
反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[C:9]2[C:4]=1[CH:5]=[N:6][NH:7][C:8]2=O.P(Cl)(Cl)([Cl:18])=O.[OH-].[Na+]>O>[Cl:18][C:8]1[C:9]2[C:4](=[C:3]([O:2][CH3:1])[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=2)[CH:5]=[N:6][N:7]=1参加物
5
実験手順
1 g (4.9 mmol) of 5,7-dimethoxy-2H-phthalazin-1-one and 10 mL of phosphoryl chloride are heated at 80° C. for 2 hours. After cooling to room temperature, the reaction medium is poured dropwise into 50 mL of water and the mixture is then basified with 6N sodium hydroxide solution and extracted with dichloromethane. The organic phase is washed with water and with brine, dried over anhydrous sodium sulfate and then evaporated under reduced pressure. 1 g of a beige-coloured solid is obtained (91% yield).
後処理
- extractionextracted with dichloromethane
- washThe organic phase is washed with water and with brine
- dry with materialdried over anhydrous sodium sulfate
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-5c9d0432b10e4a73a778c48ed2ed7938
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07423030B2
反応ノート
読み込み中…