HRID1392561
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customthe reaction mixture was quenched by NH4Cl (saturated aqueous solution)
- customthe organic phase removed in vacuo
- extractionThe aqueous phase was extracted with CHCl3
- customthe resulting two phases were separated with a phase separator (IST)
- concentrationConcentration