HRID566711

反应详情

EQUATION

反应方程式

HRID 566711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred, degassed mixture of 6-((S)-2-Amino-3-phenylpropylamino)-3-bromo-2-(4-pyridyl)pyridine (4.2 gm, 10.9 mmole), 3-methylbenzene boronic acid (1.8 gm, 13 mmole), in aqueous 2 M Na2CO3 (50 mL) and toluene (50 mL) at rt was added Pd(PPh3)4(400 mg, 0.35 mmole). The mixture was heated to reflux for 12 hrs, cooled to rt, and extracted with toluene. The combined organic layers were washed with brine, concentrated and purified (SiO2, CH2Cl2/MeOH/NH4OH: 100/11/8) to give the title compound. MS (m/z): Calcd. C26H26N4 (M+): 394, found (M+H)+: 395.1.

WORKUP

后处理

  1. customTo a stirred, degassed
  2. temperatureThe mixture was heated
  3. temperatureto reflux for 12 hrs
  4. extractionextracted with toluene
  5. washThe combined organic layers were washed with brine
  6. concentrationconcentrated
  7. custompurified (SiO2, CH2Cl2/MeOH/NH4OH: 100/11/8)