HRID1476860

反应详情

EQUATION

反应方程式

HRID 1476860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
175 °C

PROCEDURE

实验过程

To (S)-tert-butyl 3-((6-cyano-1,7-naphthyridin-8-yl)amino)pyrrolidine-1-carboxylate (210 mg, 0.619 mmol) in NMP (1.5 mL) was added ethyl hydrazinecarboxylate (258 mg, 2.475 mmol). The reaction mixture was heated at 175° C. for 2 days and was then cooled, diluted with EtOAc, and washed with aqueous NH4Cl. The organic phase was dried and concentrated. The crude product was purified by preparative HPLC eluting with a gradient of 35-60% ACN in water (acid mode) to give the title compound (80 mg, 33%).

WORKUP

后处理

  1. temperaturewas then cooled
  2. washwashed with aqueous NH4Cl
  3. customThe organic phase was dried
  4. concentrationconcentrated
  5. customThe crude product was purified by preparative HPLC
  6. washeluting with a gradient of 35-60% ACN in water (acid mode)