HRID1985407

反应详情

EQUATION

反应方程式

HRID 1985407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

30 mg of Ethyl 3-(3-amino-4-methoxyphenyl)-2-isopropoxypropanoate and 20 mg of 2,4-dichlorophenoxyacetic acid were dissolved in 0.5 ml of tetrahydrofuran, and 30 mg of carbonyldiimidazole and 0.05 ml of triethylamine were added, and the mixture was stirred at 50° C. for 4 hours. The reaction mixture was then partitioned between water and ethyl acetate, and the organic layer was concentrated. The residue was dissolved in 0.6 ml of ethanol, and 0.12 ml of 5N sodium hydroxide was added, and the mixture was stirred at room temperature for 1 hour. The reaction solution was neutralized with dilute hydrochloric acid, and extracted with ethyl acetate. The organic layer was concentrated, and the residue was purified by HPLC using a reverse-phase column and a water-acetonitrile-trifluoroacetic acid elution solvent, to give 3.4 mg of the title compound.

WORKUP

后处理

  1. customThe reaction mixture was then partitioned between water and ethyl acetate
  2. concentrationthe organic layer was concentrated
  3. dissolutionThe residue was dissolved in 0.6 ml of ethanol
  4. addition0.12 ml of 5N sodium hydroxide was added
  5. stirringthe mixture was stirred at room temperature for 1 hour
  6. extractionextracted with ethyl acetate
  7. concentrationThe organic layer was concentrated
  8. customthe residue was purified by HPLC
  9. washa water-acetonitrile-trifluoroacetic acid elution solvent