関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | L-Aspartic Acid | HCID 5960 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | L-Asparagine, monohydrate | HCID 170358 | — |
反応手順
A solution of 31.5 ml. sulfuric acid in 295 ml. methanol was treated with 66.5 g. L-aspartic acid, and heated at 40-45° C. for 4 hours. The solution was cooled to 24° C., and treated with 28% aqueous ammonia to a pH of 2.5. The mixture was concentrated under vacuum to a thick slurry. The slurry was treated with 750 ml. of 28% aqueous ammonia and 20 ml. water, and stirred at 24° C. for 3.5 hours. The mixture was concentrated under vacuum nearly to dryness, redissolved in 75 ml. water at 55° C., adjusted to pH of 5.4 with excess ammonia, and then cooled to 24° C. The solid was collected by filtration, washed and dried, and finally recrystallized from another 75 ml. water to yield 31.0 g asparagine monohydrate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05326908 |
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| 出典データセット | uspto-grants-1994_07 |
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| ORD ID | ord-d0326cd7a0e74954b3cf17c531e61e0a |
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| 出典メモ | uspto-grants-1994_07 |
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