関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Dimethylphenylsilane | HCID 13014 | — |
| 反応物 | O-benzylbenzaldoxime | HCID 561973 | — |
| 生成物 | N-(Benzyloxy)-1-phenylmethanamine--hydrogen chloride (1/1) | HCID 18358890 | 45% |
反応手順
To a solution of crude N-benzyloxybenzylideneamine from Example 22(a) (3.0 g, 14.2 mmol) in dichloromethane (30 mL) at 0° C. was added dimethylphenylsilane (3.09 mL, 20.3 mmol) followed by trifluoroacetic acid (3.92 mL, 50.6 mmol). The solution was allowed to warm to room temperature and was stirred for 16 hours. The solution was concentrated by rotary evaporation. To the crude oil was added dichloromethane (20 mL) and a hydrogen chloride saturated solution of dichloromethane (20 mL). The insoluble material (300 mg) was filtered and the solution was concentrated by rotary evaporation. To the crude oil was added a hydrogen chloride saturated solution of ether (20 mL). Additional ether (100 mL) was added and the insoluble material was filtered. The solid obtained was combined with the initial solid filtered above to give the title compound (1.57 g, 45%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06124281 |
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| 出典データセット | uspto-grants-2000_09 |
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| ORD ID | ord-bbc888ece2df40b6954a4ea0c418b91f |
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| 出典メモ | uspto-grants-2000_09 |
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