化工社化工社 化学情報印刷レポート · 研究参考用
Benzyl chloroformate → Benzyl 3-bromopropylcarbamate
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 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | Benzyl 3-bromopropylcarbamate | HCID 254436 | 105.3% |
反応手順
Benzylchloroformate (8.6 ml, 60 mmol) was added to a stirred mixture of 3-bromopropylamine hydrobromide (6.6 g, 30 mmol) in methylene chloride (100 ml) and 3N sodium hydroxide solution (100 ml) at 0° C. After stirring two phase reaction mixture at room temperature for overnight, organic layer was separated and washed with water twice (30 ml×2). After drying with MgSO4, the volatile solvent was evaporated under reduced pressure. The residue was purified with silica gel column chromatography (EtOAc:Hx=1:4) to obtain desire compound (8.6 g, 98%) as colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895558B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-8d5f0cc8a2fd49aa9f4c3dc927ecccc8 |
| 出典メモ | uspto-grants-2014_11 |