関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Bromoisoquinoline | HCID 736487 | — |
| 反応物 | 2-(Di-tert-butylphosphino)biphenyl | HCID 2734215 | — |
| 反応物 | tert-butyl N-(3-aminopropyl)-N-methylcarbamate | HCID 2756543 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(tert-butoxycarbonyl)-N-methyl-N'-(5-isoquinolyl)-1,3-propylenediamine | HCID 21979883 | 85.1% |
反応手順
Under nitrogen atmosphere, a suspension of 5-bromoisoquinoline (252 mg), tris(dibenzylideneacetone)palladium(0) (59 mg), 2-(di-tert-butylphosphino)biphenyl (74 mg), (3-aminopropyl)methylcarbamic acid tert-butyl ester (274 mg, Asta Tech), and sodium tert-butoxide (163 mg) in toluene was stirred with heating at 70° C. for 3 hours. The reaction mixture was returned to room temperature and purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1) to obtain the title compound (325 mg).
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-34859159c1f24492b072bc7bfbc36a45 |
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| 出典メモ | uspto-grants-2006_08 |
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