関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Carbonic acid, bis(2-methylpropyl) ester | HCID 68321 | — |
| 生成物 | N-Benzylacetamide | HCID 11500 | — |
反応手順
After completion of the reaction, 1% hydrochloric acid (23 g) was dropwide added at 10° C. or lower and after stirred for 30 minutes, settled and separated. The obtained organic layer was washed with 9% salt water (7 g) at 5 to 10° C., settled and separated. The obtained organic layer was washed with an aqueous 5% sodium hydrogen carbonate solution (11.8 g) at 15 to 30° C., settled and separated. After that, the organic layer was washed with ion-exchange water (6 g) at 25 to 35° C., settled and separated. The obtained organic layer was evaporated to obtain a solution (10.04 g) of a desired pale yellowish transparent solution or white solid. The content was found 86.5% by gas chromatography analysis. The pure product yield was 8.68 g (yield 87.8% based on acetic acid). The content of impurities are as follows: diisobutylcarbonate: 2.0%, and N-isobutyloxycarbonyl)-benzylamine: 2.5%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06927290B2 |
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| 出典データセット | uspto-grants-2005_08 |
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| ORD ID | ord-02496331e15b47e6bb3822a1b43eac57 |
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| 出典メモ | uspto-grants-2005_08 |
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