関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Glyoxylic Acid | HCID 760 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | (Cyanomethyl)urea | HCID 80065 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Orotic Acid | HCID 967 | 71.8% |
反応手順
A suspension of 57 g of cyanomethylurea in 45 ml of methanol is heated to boiling under agitation, combined with 3 ml of 8N sodium hydroxide solution, and heated under reflux for 30 minutes. The reaction mixture is then allowed to cool down to 30° C., 550 ml of water and 90 g of 50% strength glyoxylic acid are added thereto, and the mixture is neutralized with 8N sodium hydroxide solution at a temperature of maximally 30° C. until a pH of 6.5 has been attained. The mixture is then heated to 55°-60° C., 225 ml of 8N sodium hydroxide solution is added dropwise thereto at this temperature within one hour, and the mixture is stirred for another 2 hours. Then about 150 ml of aqueous methanol is removed by distillation to 95° C.; the mixture is heated for one hour under reflux and gently acidified with concentrated nitric acid. The mixture is allowed to cool down to room temperature, the thus-separated crystallized product is filtered off, washed with water, and dried under vacuum, thus obtaining 72 g of orotic acid (=71.8% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04734506 |
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| 出典データセット | uspto-grants-1988_03 |
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| ORD ID | ord-c7731ea97c854d9281812ac0cf8d3e2c |
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| 出典メモ | uspto-grants-1988_03 |
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