参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 三乙胺 | HCID 8471 | — |
| 反应物 | 2,4-二氯-7-甲基噻吩并[3,2-D]嘧啶 | HCID 7147064 | — |
| 反应物 | BETA-丙胺酰胺盐酸盐 | HCID 22222288 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | 2-Chloro-4-(2-carbamoylethylamino)-7-methylthieno[3,2-d]pyrimidine | HCID 18326411 | 79.8% |
反应步骤
In 10 ml of DMF, 1.0 g (4.9 mmol) of 2,4-dichloro-7-methylthieno[3,2-d]pyrimidine was dissolved, and then 668 mg (5.37 mmol) of β-alanineamide hydrochloride and 1.09 g (10.7 mmol) of triethylamine were added thereto under ice cooling. The reaction solution was stirred at 0° C. for one hour and then allowed to resume room temperature, followed by stirring for further 1 hour. After completion of the reaction, ice water was added to the reaction mixture, followed by extraction with ethyl acetate (50 ml×3). After the organic layer was washed successively with 1N hydrochloric acid, water and brine and dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/8) to give 1.05 g (yield: 79.8%) of the title compound.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US06339089B2 |
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| 来源数据集 | uspto-grants-2002_01 |
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| ORD ID | ord-064543062e254504b9e2a0586f065070 |
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| 来源说明 | uspto-grants-2002_01 |
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