HRID2234477

反应详情

EQUATION

反应方程式

HRID 2234477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl1-[(propan-2-ylamino)methyl]cyclopropane-1-carboxylate (Intermediate 211; 9.55 g, 50 mmol) in acetone (300 mL) was added potassium carbonate (7.05 g, 51 mmol) followed by 2,4-dichloro-5-nitropyrimidine (Aldrich; 10.675 g, 55 mmol). The mixture was stirred overnight at room temperature, concentrated in vacuo and partitioned between EtOAc and water. The EtOAc layer was separated, dried over sodium sulfate, then purified by column chromatography (EtOAc/isohexane 10:90), to yield the title compound as a yellow oil. (11 g, 64%)

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. custompartitioned between EtOAc and water
  3. customThe EtOAc layer was separated
  4. dry with materialdried over sodium sulfate
  5. custompurified by column chromatography (EtOAc/isohexane 10:90)