HRID391620

反应详情

EQUATION

反应方程式

HRID 391620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 2-chloro-6-(2-methoxyphenylamino)-5-nitropyrimidine-4-carboxylate. In a 250 mL round-bottomed flask was placed ethyl 2,6-dichloro-5-nitropyrimidine-4-carboxylate (2 g, 7.52 mmol) in tetrahydrofuran (50 mL) and the mixture was cooled down to −78° C. A solution of 2-methoxyaniline (0.763 mL, 6.77 mmol) and diisopropylethyl amine (1.313 mL, 7.52 mmol) in 4 mL of tetrahydrofuran was added dropwise and the reaction was allowed to warm to room temperature overnight. Solvent was removed under reduced pressure and the crude material was purified by column chromatography (SiO2, 90% nHexanes in ethyl acetate) to provide the title compound as an orange solid (2.42 g, 6.86 mmol, 91% yield). MS (ESI) m/z 353.3 [M+1]+.

WORKUP

后处理

  1. customIn a 250 mL round-bottomed flask was placed
  2. customSolvent was removed under reduced pressure
  3. customthe crude material was purified by column chromatography (SiO2, 90% nHexanes in ethyl acetate)