Dimethylformamide → HCID 58484329、化合物
反応式
[CH3:1][N:2]1[C:7](=[O:8])[CH:6]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)[CH:4]=[N:3]1.O=P(Cl)(Cl)Cl.CN([CH:24]=[O:25])C>>[CH3:1][N:2]1[C:7](=[O:8])[C:6]([CH:24]=[O:25])=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)[CH:4]=[N:3]1参加物
実験手順
A solution of 2-methyl-5-(4-methylpiperazin-1-yl)pyridazin-3(2H)-one (416 mg, 2 mmol) in dry DMF (6.7 ml) was cooled to 5° C., then a solution of POCl3 (0.41 ml, 4.4 mmol) in dry DMF (1 ml) was added dropwise. The cooling bath was removed and the mixture was stirred at room temperature for 10 min. Then, the temperature was raised to 70° C. and stirring was continued for 75 min. After cooling, the volatile components were removed under reduced pressure and the residue was treated with crushed ice (15 g). The mixture was adjusted to pH 7-8 with aqueous NaOH. Then it was extracted with dichloromethane (4×40 ml) and the combined extracts were washed with water, dried (Na2SO4) and evaporated. Residual volatile material was removed at 10−2 mbar to leave an oily residue which slowly solidified on storage in a refrigerator.
後処理
- customThe cooling bath was removed
- temperatureThen, the temperature was raised to 70° C.
- stirringstirring
- waitwas continued for 75 min
- temperatureAfter cooling
- customthe volatile components were removed under reduced pressure
- additionthe residue was treated with crushed ice (15 g)
- extractionThen it was extracted with dichloromethane (4×40 ml)
- washthe combined extracts were washed with water
- dry with materialdried (Na2SO4)
- customevaporated
- customResidual volatile material was removed at 10−2 mbar
- customto leave an oily residue which
出典と根拠
- ORDレコード
- ord-0517fd94e77046c48ae04301588d9801
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536210B2
反応ノート
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