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Methanol → 1-Acetyl-2-methoxyhexahydroazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1-(Azepan-1-yl)ethan-1-one | HCID 22059 | — |
| 触媒 | Tetramethylammonium tetrafluoroborate | HCID 12621 | — |
| 生成物 | 1-Acetyl-2-methoxyhexahydroazepine | HCID 14761782 | 90.3% |
反応手順
In the same manner as indicated in Example 6 there are electrolyzed 23.2 g of N-acetylhexahydroazepine and 57.7 g of methanol in the presence of 0.26 g of tetramethylammonium tetrafluoroborate as conducting salt. After throughput of 2.5 Faraday per mol of N-acetylhexahydroazepine the current is switched off. The calculated mean cell voltage is 40.8 volts. Work-up of the electrolysis solution gives 25.4 g of 1-acetyl-2-methoxyhexahydroazepine (boiling point 53° C./0.06 mbar; nD25 = 1.4775), which corresponds to a product yield of 90.1% and a current efficiency of 71.5%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04118500 |
| 出典データセット | uspto-grants-1978_10 |
| ORD ID | ord-0004027a6650406698c209fa2b2ee757 |
| 出典メモ | uspto-grants-1978_10 |