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三氟乙酸 → (2R)-3-(1,1'-biphenyl-4-yl)-N-methyl-2-methylamino-N-((1R)-1-methylcarbamoyl-2-phenylethyl)propionamide
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 三氟乙酸 | HCID 6422 | — |
| 反应物 | 碳酸氢三钠 | HCID 10791 | — |
| 反应物 | 碳酸氢钠 | HCID 516892 | — |
| 反应物 | ((1R)-2-(1,1'-Biphenyl-4-yl)-1-(methyl-((1R)-1-(methylcarbamoyl)-2-phenylethyl)carbamoyl)ethyl)methyl-carbamic acid tert-butylester | HCID 10530245 | — |
| 溶剂 | 二氯甲烷 | HCID 6344 | — |
| 产物 | (2R)-3-(1,1'-biphenyl-4-yl)-N-methyl-2-methylamino-N-((1R)-1-methylcarbamoyl-2-phenylethyl)propionamide | HCID 10812511 | 98.3% |
反应步骤
((1R)-2-(1,1'-Biphenyl-4-yl)-1-(methyl-((1R)-1-(methylcarbamoyl)-2-phenylethyl)-carbamoyl)ethyl)methyl-carbamic acid tert-butylester (1.0 g; 1.8 mmol) was dissolved in methylene chloride (4 mL). Trifluoroacetic acid (4 mL) was added and the reaction mixture was stirred for 15 min at room temperature. Methylene chloride (40 mL), an aqueous solution of sodium hydrogen carbonate/sodium carbonate (pH 9; 40 mL) and sodium hydrogen carbonate (solid) were added to the reaction mixture until pH 9. The organic phase was dried (magnesium sulfate) and the solvent was removed in vacuo to afford 0.76 g of (2R)-3-(1,1'-biphenyl-4-yl)-N-methyl-2-methylamino-N-((1R)-1-methylcarbamoyl-2-phenylethyl)propionamide.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US06127391 |
| 来源数据集 | uspto-grants-2000_10 |
| ORD ID | ord-1af3dd60570a4617b11cb3134442c4cb |
| 来源说明 | uspto-grants-2000_10 |