HRID8455

反应详情

EQUATION

反应方程式

HRID 8455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

Methyl (2R)-2-(2,3,4-trifluoroanilino)propionate (223 mg, 91% ee) was dissolved in DMAc (3 ml) and potassium carbonate (474.1 mg) was added thereto at room temperature. The liquid reaction mixture was stirred at 95° C. for 19 hours. After adding an aqueous solution of sodium hydroxide (3 mol/l), the liquid reaction mixture was stirred for 1 hour and then adjusted to pH 2 with hydrochloric acid (3 mol/l) followed by extraction with IPE. Next, it was dried over anhydrous magnesium sulfate. After evaporating the solvent, the crude product thus obtained was recrystallized from a solvent mixture of methylene chloride with normal hexane to thereby give the title compound (198 mg) as colorless crystals. The optical purity of this product was 0% ee. Various spectral data of this product was identical with those obtained in Example 23.

WORKUP

后处理

  1. customat room temperature
  2. customThe liquid reaction mixture
  3. customthe liquid reaction mixture
  4. stirringwas stirred for 1 hour
  5. extractionfollowed by extraction with IPE
  6. dry with materialNext, it was dried over anhydrous magnesium sulfate
  7. customAfter evaporating the solvent
  8. customthe crude product thus obtained
  9. customwas recrystallized from a solvent mixture of methylene chloride with normal hexane