HRID2300895

反应详情

EQUATION

反应方程式

HRID 2300895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2-[(S)-1-phenylethylamino]-4-[5-aminobenzimidazol-1-yl]pyrimidine (49.8 mg) was dissolved in DMF (2 mL). Diisopropylethylamine (79 μL) and 4-bromopyridine hydrochloride (43.2 mg) were added, and the mixture left heating overnight at 100° C. After 17 h added more diisopropylethylamine (79 μL) and 4-bromopyridine hydrochloride (40.2 mg) and continued heating at 100° C. for another 24 h. The volatiles were removed in vacuo and the residue purified on silica gel (2-5%(2M NH3 in MeOH)/CH2Cl2) to yield 5.0 mg of impure product that was purified by HPLC (Zorbax Rx-SIL, 60:40 hexanes:ethanol) to yield 3.0 mg of the title compound. Mass spectrum (ESI) 408.4 (M+1).

WORKUP

后处理

  1. waitthe mixture left
  2. temperaturecontinued heating at 100° C. for another 24 h
  3. customThe volatiles were removed in vacuo
  4. customthe residue purified on silica gel (2-5%(2M NH3 in MeOH)/CH2Cl2)