関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 3-Bromopropylamine hydrobromide | HCID 78701 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | (3-Aminopropyl)(triphenyl)phosphonium dibromide | HCID 131737002 | 117.3% |
反応手順
To a stirred, degassed solution of 3-bromopropylamine hydrobromide (25.1 g, 115 mmol) in 1-butanol (210 mL) was added triphenylphosphine (42.1 g, 160 mmol). The solution was degassed again by bubbling nitrogen through it for 10 minutes and then heated at 120° C. overnight. The solution was cooled and poured into a stirring solution of methyl t-butyl ether (700 mL) and toluene (400 mL). After stirring at room temperature until a homogenous slurry resulted, the solids were filtered and the product cake rinsed two times with methyl t-butyl ether (2×100 mL) to afford the title compound (54 g, 84%), as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434753B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-ce9b76e83a664bd783d6cfab82c42e45 |
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| 出典メモ | uspto-grants-2016_09 |
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