反応式
[CH3:1][C:2]1[S:3][C:4]([CH3:23])=[CH:5][C:6]=1[C:7]1[N:8]=[C:9]2[N:13]([C:14]=1[CH2:15][C:16]([OH:18])=O)[C:12]1[CH:19]=[CH:20][CH:21]=[CH:22][C:11]=1[S:10]2.[CH3:24][NH2:25]>O1CCCC1>[CH3:1][C:2]1[S:3][C:4]([CH3:23])=[CH:5][C:6]=1[C:7]1[N:8]=[C:9]2[N:13]([C:14]=1[CH2:15][C:16]([NH:25][CH3:24])=[O:18])[C:12]1[CH:19]=[CH:20][CH:21]=[CH:22][C:11]=1[S:10]2参加物
反応条件
- 温度
- 0 °C
実験手順
A solution of 1.5 g (0.0044 mole) of 2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetic acid in 30 ml of anhydrous tetrahydrofuran is treated, at room temperature, with 0.85 g (0.005 mole) of N,N'-carbonyldiimidazole for 30 minutes. The solution which has become clear is cooled to 0° C. and a stream of methylamine is passed through it for 30 minutes. The mixture is allowed to return to room temperature, the stirring is continued for 3 h, the solvent is evaporated under reduced pressure, the residue is taken up in 10 ml of water, it is extracted with dichloromethane, the organic phase is separated, it is washed with water, it is dried over sodium sulphate, the solvent is evaporated under reduced pressure, and the residue is crystallized from ethyl acetate. 1 g of pale yellow crystals is finally obtained. Melting point: 238°-239° C.
後処理
- customto return to room temperature
- customthe solvent is evaporated under reduced pressure
- extractionit is extracted with dichloromethane
- customthe organic phase is separated
- washit is washed with water, it
- dry with materialis dried over sodium sulphate
- customthe solvent is evaporated under reduced pressure
- customthe residue is crystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-7156c0337bdd40d492d7eeed097f1fac
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05418248
関連ノート
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