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Sulfuric Acid → HCID 54211560、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Isobutylene | HCID 8255 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | (2S)-2-Amino-4,4-dimethylpentanoic acid | HCID 194032 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 54211560 | HCID 54211560 | 50.5% |
反応手順
To a pressure bottle were added 1.5 gm (10.3 mMol) 4-methyl-(L)-leucine, 25 mL dioxane, 1.5 mL concentrated sulfuric acid and 25 mL isobutylene. The pressure bottle was stoppered and the reactants were shaken together for 18 hours. The reaction mixture was then treated with 60 mL cold 1N sodium hydroxide and 100 mL ethyl acetate. To this mixture was added sufficient 1N sodium hydroxide until the pH of the mixture was 8.5. The layers were separated and the aqueous phase was extracted well with ethyl acetate. The combined ethyl acetate phases were dried over sodium sulfate and concentrated under reduced pressure to provide an oil which gradually crystallized to provide 1.05 gm (50.5%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06521611B2 |
| 出典データセット | uspto-grants-2003_02 |
| ORD ID | ord-0e46048ccc6f4d8d8616456547e2fb54 |
| 出典メモ | uspto-grants-2003_02 |