HRID391628

反应详情

EQUATION

反应方程式

HRID 391628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 2-(3-hydroxyphenylamino)-6-(2-methoxyphenylamino)-5-nitropyrimidine-4-carboxylate. To a solution of ethyl 2-chloro-6-(2-methoxyphenylamino)-5-nitropyrimidine-4-carboxylate (See Example 30.A) (200 mg, 0.567 mmol) in DMF (3 mL) was added 3-aminophenol (74.3 mg, 0.680 mmol) and N,N-diisopropylethylamine (0.149 mL, 0.851 mmol). The reaction was stirred at room temperature overnight. Solvent was removed under reduced pressure and the resulting residue was purified by chromatography on a normal phase silica gel column (25-43% ethyl acetate in hexanes). Fractions containing product were combined and the solvent evaporated to provide the title compound (227 mg, 0.534 mmol, 94% yield) as an orange solid. MS (ESI) m/z 426.2 [M+1]+.

WORKUP

后处理

  1. customSolvent was removed under reduced pressure
  2. customthe resulting residue was purified by chromatography on a normal phase silica gel column (25-43% ethyl acetate in hexanes)
  3. additionFractions containing product
  4. customthe solvent evaporated