関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (2S)-2-Amino-4,4-dimethylpentanoic acid | HCID 194032 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 2-Hydroxy-4,4-dimethylpentanoic acid | HCID 22709417 | — |
反応手順
805 mg (5.54 mmol) of 4-methylleucine (racemate) were initially charged in 11 ml of sulphuric acid (1M) and cooled to 0° C. 2.30 g (33.3 mmol) of sodium nitrite as a solution in 6.5 ml of water were then slowly added dropwise over a period of 90 min. The solution was stirred at RT for another 24 h. The mixture was carefully diluted with 10 ml of water and the aqueous phase was extracted five times with 10 ml of methyl tert-butyl ether. The combined organic phases were washed with 25 ml of saturated aqueous sodium chloride solution, dried over sodium sulphate and filtered, and the solvent was removed under reduced pressure. The crude product was used for the next step without further purification. Yield: 667 mg (82% of theory)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434690B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-d72472775a0a461a8daa0768d46eef91 |
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| 出典メモ | uspto-grants-2016_09 |
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