関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | tert-Butyl (3-aminopropyl)carbamate | HCID 2735700 | — |
| 反応物 | 5-Isoquinolinesulfonyl chloride | HCID 3371655 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-1,3-propylenediamine | HCID 21979958 | — |
反応手順
A solution of N-(tert-butoxycarbonyl)-1,3-propylenediamine (2.09 g, Tokyo Kasei Kogyo) and triethylamine (3.4 ml, Tokyo Kasei Kogyo) in dichloromethane (20 ml) was added with a solution of isoquinoline-5-sulfonyl chloride (2.73 g, prepared according to Japanese Patent Unexamined Publication (Kokai) No. 61-227581) in dichloromethane (15 ml) with stirring and ice cooling and stirred at room temperature for 14 hours and 30 minutes. The reaction mixture was washed successively with saturated aqueous sodium hydrogencarbonate and saturated brine. The organic layer was dried, and then the solvent was evaporated under reduced pressure. Then, the residue was purified by flash column chromatography (chloroform:methanol=50:1) to obtain the title compound (4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07094789B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-e7e86c6093174ea1bac2f28462d3f752 |
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| 出典メモ | uspto-grants-2006_08 |
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