HRID1392561

反应详情

EQUATION

反应方程式

HRID 1392561 的结构方程式

PROCEDURE

实验过程

To a stirred solution of 4-(4-amino-2,6-dibromo-3-methylphenoxy)-2-hydroxymethyl-6-isopropylphenol of Part 10B (18 mg, 0.04 mmol), ethylmalonylchloride (5.7 μl, 0.044 mmol) and THF (0.5 mL) was added Et3N (11 μl, 0.08 mmol). After 2 hours stirring at room temperature, the reaction mixture was quenched by NH4Cl (saturated aqueous solution) and the organic phase removed in vacuo. The aqueous phase was extracted with CHCl3 and the resulting two phases were separated with a phase separator (IST). Concentration gave 22 mg (98%) of N-[3,5-dibromo-4-[4-hydroxy-3-hydroxymethyl-5-isopropylphenoxy]-2-methylphenyl]malonamic acid ethyl ester as a yellow foam.

WORKUP

后处理

  1. customthe reaction mixture was quenched by NH4Cl (saturated aqueous solution)
  2. customthe organic phase removed in vacuo
  3. extractionThe aqueous phase was extracted with CHCl3
  4. customthe resulting two phases were separated with a phase separator (IST)
  5. concentrationConcentration