三氟乙酸 → (2R)-3-(4-fluorophenyl)-N-methyl-2-methylaminopropionamide

HRID 366199

反应方程式

HRID 366199 反应方程式
C(O[C:6](=O)[N:7]([C@@H:9]([C:18](=[O:21])[NH:19][CH3:20])[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=1)C)(C)(C)C.FC(F)(F)C(O)=O.C(=O)([O-])O.[Na+].C(=O)([O-])[O-].[Na+].[Na+].C(=O)([O-])O.[Na+]>C(Cl)Cl>[F:17][C:14]1[CH:13]=[CH:12][C:11]([CH2:10][C@@H:9]([NH:7][CH3:6])[C:18]([NH:19][CH3:20])=[O:21])=[CH:16][CH:15]=1

参与物

6

反应物 4

HCID 6422三氟乙酸HCID 10791碳酸氢三钠HCID 516892碳酸氢钠HCID 10828758((1R)-2-(4-fluorophenyl)-1-(methylcarbamoyl)ethyl)-methylcarbamic acid tert-butylester

产物 1

HCID 10560386(2R)-3-(4-fluorophenyl)-N-methyl-2-methylaminopropionamide收率 91.6%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

实验过程

((1R)-2-(4-Fluorophenyl)-1-(methylcarbamoyl)ethyl)-methylcarbamic acid tert-butylester (1.0 g; 3.22 mmol) was dissolved in methylene chloride (5 mL). Trifluoroacetic acid (5 mL) was added and the reaction mixture was stirred for 30 min at room temperature. Methylene chloride (30 mL), an aqueous solution of sodium hydrogen carbonate/sodium carbonate (pH 9; 30 mL) and sodium hydrogen carbonate (solid), were added to the reaction mixture, until pH 9. The organic phase was dried (magnesium sulfate) and evaporated in vacuo to afford 0.62 g of (2R)-3-(4-fluorophenyl)-N-methyl-2-methylaminopropionamide.

后处理

  1. dry with materialThe organic phase was dried (magnesium sulfate)
  2. customevaporated in vacuo

来源与证据

ORD记录
ord-228cdf3778064460a58a54f65a9f0d1a
来源数据集
uspto-grants-2000_10
专利号
US06127391

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