関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(Diphenylmethyl)azetidin-3-ol | HCID 330448 | — |
| 触媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(Benzyloxy)-1-(diphenylmethyl)azetidine | HCID 16089448 | 24.3% |
反応手順
To a solution of 1-diphenylmethylazetidin-3-ol (300 mg, 1.3 mmol) in DMF (2.6 mL) at 0° C. under nitrogen was added NaH (60% in oil, 56 mg, 1.4 mmol). The suspension was stirred for 0.5 h at 0° C. then treated with benzyl bromide (236 μL, 2.0 mmol). The mixture was allowed to warm to room temperature then heated to 80° C. overnight. The reaction mixture was cooled, acetic acid (20 drops) was added and the mixture concentrated under reduced pressure. The crude material was purified on column chromatography (eluent: Pentane/EtOAc, 95/5 to 70/30) to give the product (104 mg, 24%) as an orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08846711B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-df8f8c4729084f1e89502c2b257a43f8 |
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| 出典メモ | uspto-grants-2014_09 |
|---|
