関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | p-Nitrobenzaldoxime | HCID 96339 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Aminobenzylamine | HCID 427814 | 92.1% |
反応手順
33.2 g (0.2 mol) of this p-nitrobenzaldoxime, 18.3 g (0.25 mol) of boric anhydride, 1 g of a 5% Pt-C catalyst and 100 ml of methanol were charged into a hermetically sealed glass container and vigorously stirred while charging hydrogen. Reaction was continued at temperatures of 25° C. to 30° C. for 13.5 hours and 22.2 l of hydrogen was absorbed. Next, this reaction mixture was filtered to remove the catalyst and methanol was distilled off by concentration under reduced pressure. A yellow viscous liquid thus obtained was neutralized by adding 57 g (0.5 mol) of a 35% aqueous solution of sodium hydroxide and then, the liquid was separated to two layers. The lower layer, a colorless and transparent aqueous solution of sodium borate was removed and then, a brown and oily crude p-aminobenzylamine was obtained. This crude p-aminobenzylamine was subject to vacuum distillation at pressure of 5 to 6 mmHg and 22.5 g of fractions between 129.5° C. and 130° C. was obtained (yield 92.1%). The purity by means of gas chromatography was 99.93%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04751328 |
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| 出典データセット | uspto-grants-1988_06 |
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| ORD ID | ord-3829e8c76de8498ebb97cdb48cb411da |
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| 出典メモ | uspto-grants-1988_06 |
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