HRID969688

反应详情

EQUATION

反应方程式

HRID 969688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 2-amino-N-(4-tert-butyl-phenyl)-benzamide (Step A, 163 mg, 0.61 mmol), 2-chloro-[1,7]naphthyridine (100 mg, 0.61 mmol), Pd2(dba)3 (6.0 mg, 0.006 mmol), 2-dicyclohexyl phosphino-2′-(N-N-dimethyamino)biphenyl (6.0 mg, 0.015 mmol), and LiN(TMS)2 (1 M solution in THF, 2.3 mL) was heated at 80° C. for 12 h in a sealed tube. The mixture was concentrated in vacuo and the crude material was purified with flash chromatography (SiO2, 20% EtOAc/hexane) and crystallization from EtOH to give the desired compound. MS (ES+): 397.0 (M+H)+. Calc'd for C25H24N4O-396.48.

WORKUP

后处理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe crude material was purified with flash chromatography (SiO2, 20% EtOAc/hexane) and crystallization from EtOH