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HRID 1986188作成日:2026年10月26日

Hydrochloric Acid → 2-{5-Methyl-2-[3-(4-methyl-piperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid tri-hydrochloride

https://huagongshe.com/reaction/1986188

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物Lithium HydroxideHCID 3939—
反応物TetrahydrofuranHCID 8028—
反応物2-{5-Methyl-2-[3-(4-methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid methyl esterHCID 68857060—
溶媒MethanolHCID 887—
溶媒WaterHCID 962—
生成物2-{5-Methyl-2-[3-(4-methyl-piperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid tri-hydrochlorideHCID 6885480397%

反応条件

温度70 °C

反応手順

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].

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07547691B2
出典データセットuspto-grants-2009_06
ORD IDord-2b16bcd0d7d6427ba05d937de4fc4041
出典メモuspto-grants-2009_06