反応式
[H-].[Na+].[OH:3][CH2:4][C:5]([CH3:12])([CH3:11])[CH2:6][S:7]([NH2:10])(=[O:9])=[O:8].Cl[C:14]1[CH:15]=[CH:16][C:17]2[N:18]([N:20]=[CH:21][N:22]=2)[N:19]=1.Cl>CN(C)C=O.O>[CH3:11][C:5]([CH3:12])([CH2:6][S:7](=[O:9])(=[O:8])[NH2:10])[CH2:4][O:3][C:14]1[CH:15]=[CH:16][C:17]2[N:18]([N:20]=[CH:21][N:22]=2)[N:19]=1参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
In 15 ml of dimethylformamide was suspended 0.42 g of 60% sodium hydride in oil, followed by addition of 0.878 g of 3-hydroxy-2,2-dimethyl-1-propanesulfonamide and the mixture was stirred under reduced pressure at room temperature for 30 minutes. Then, 0.773 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added and the mixture was further stirred at room temperature for 1 hour. Following addition of 40 ml of iced water, the reaction mixture was adjusted to pH 6 with 1N-hydrochloric acid and the resulting crystals were collected by filtration and washed with 20 ml of water and 20 ml of ethyl ether. The washed crystals were recrystallized from hot ethanol to provide 1.16 g of the title compound. m.p. 181°-184° C.
後処理
- stirringthe mixture was further stirred at room temperature for 1 hour
- filtrationthe resulting crystals were collected by filtration
- washwashed with 20 ml of water and 20 ml of ethyl ether
- customThe washed crystals were recrystallized from hot ethanol
出典と根拠
- ORDレコード
- ord-6bbeb6dddcf6462faf560fd81a923fba
- 出典データセット
- uspto-grants-1995_02
- 特許番号
- US05389633
関連ノート
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