化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → (S)-2-amino-4-methyl-pentanoic acid [1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-yl]amide hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | {(S)-1-[1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-ylcarbamoyl]-3-methyl-butyl}-carbamic acid t-butyl ester | HCID 67504285 | — |
| 生成物 | (S)-2-amino-4-methyl-pentanoic acid [1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-yl]amide hydrochloride | HCID 66899584 | 100% |
反応手順
A solution of {(S)-1-[1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-ylcarbamoyl]-3-methyl-butyl}-carbamic acid t-butyl ester (4.15 g) in dichloromethane (8 mL) was treated with trifluoroacetic acid (8 mL) and stirred at room temperature for 1 h. At this time the mixture was concentrated in vacuo and the residue dissolved in methanol (10 mL) and treated with hydrogen chloride gas for 2 min. The mixture was concentrated in vacuo and the residue was dried under high vacuum. The solid obtained was triturated with diethyl ether which afforded (S)-2-amino-4-methyl-pentanoic acid [1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-yl]amide hydrochloride (3.86 g, 100%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741327B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-152031cee96541c2bd021b434ddece9f |
| 出典メモ | uspto-grants-2010_06 |