反応式
C[O:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[CH:12]=[C:11]([C:13]3[C:18]([CH3:19])=[CH:17][N:16]=[C:15]([NH:20][CH2:21][CH2:22][CH2:23][N:24]4[CH2:29][CH2:28][N:27]([CH3:30])[CH2:26][CH2:25]4)[N:14]=3)[S:10][C:9]=2[CH:31]=1)=[O:4].C1COCC1.[OH-].[Li+].[ClH:39]>CO.O>[ClH:39].[ClH:39].[ClH:39].[CH3:19][C:18]1[C:13]([C:11]2[S:10][C:9]3[CH:31]=[C:5]([C:3]([OH:4])=[O:2])[CH:6]=[CH:7][C:8]=3[CH:12]=2)=[N:14][C:15]([NH:20][CH2:21][CH2:22][CH2:23][N:24]2[CH2:25][CH2:26][N:27]([CH3:30])[CH2:28][CH2:29]2)=[N:16][CH:17]=1参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 70 °C
実験手順
2-{5-Methyl-2-[3-(4-methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid methyl ester (1.31 g, 2.98 mmol) is dissolved in methanol (30 mL), THF (30 mL) and water (10 mL) and lithium hydroxide solution (4.6 mL of 2.0 M solution) is added. The solution is heated at 70° C. for 4.5 hours and 5 N HCl (9 mL) is added in one portion while still heating the solution. The solution is cooled to room temperature and the resulting solid is filtered and washed with methanol. The solid is dried at 60° C. in a vacuum oven for 4 hours to give the title compound (1.43 g, 97% yield). ES+(m/z) 426 [M+H].
後処理
- temperaturewhile still heating the solution
- temperatureThe solution is cooled to room temperature
- filtrationthe resulting solid is filtered
- washwashed with methanol
- customThe solid is dried at 60° C. in a vacuum oven for 4 hours
出典と根拠
- ORDレコード
- ord-2b16bcd0d7d6427ba05d937de4fc4041
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07547691B2
関連ノート
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