関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | 3-Bromopropylamine hydrobromide | HCID 78701 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Benzyl 3-bromopropylcarbamate | HCID 254436 | 62.7% |
反応手順
To a stirred suspension of 3-bromopropylamine hydrobromide (2 g, 9.14 mM) in 40 mL dry THF was added, via hypodermic syringe, benzyl chloroformate (1.64 g, 9.60 mM) at room temperature. After cooling to 0° C., diisopropylethylamine (1.6 mL, 9.20 mM) was added dropwise via syringe and the reaction mixture was allowed to stir at 0° C. for 1 hour. The crude reaction mixture was filtered over a pad of Celite and solvents were evaporated. The residue was flash chromatographed on silica gel, eluting with 10-20-30% EtOAc/hexane to afford 1.56 g desired product as a liquid, homogeneous by TLC in 80:20 hexane-EtOAc;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05411980 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-e1b2cbc13a4d4e269a66fa91b9949ec9 |
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| 出典メモ | uspto-grants-1995_05 |
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