HRID595852

反应详情

EQUATION

反应方程式

HRID 595852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To 3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)cyclopent-2-enone (2.99 g, 14.37 mmol) (the filtrate from last step) was added 2-amino-5 bromopyrazine (2.5 g, 14.37 mmol), PdCl2(dppf)-CH2Cl2 (1.173 g, 1.437 mmol), Na2CO3 (7.61 g, 71.8 mmol) and water (17.96 mL) the reaction mixture was stirred at 100° C. oil bath for overnight, filtered through Celite. The reaction mixture was then extracted by EtOAc. The organic was then used 3N HCl (20 mL) washed 2 times, and water 50 mL once, the AQ was then neutralized by NaOH to pH=8, the reaction mixture was then extracted by CHCl3/IPA (7:3) 3 times, the organic was dried and concentrated and used as it. LCMS (m/z): 176.1 (MH+), 0.32 min.

WORKUP

后处理

  1. filtrationfiltered through Celite
  2. extractionThe reaction mixture was then extracted by EtOAc
  3. washwashed 2 times, and water 50 mL once
  4. extractionthe reaction mixture was then extracted by CHCl3/IPA (7:3) 3 times
  5. customthe organic was dried
  6. concentrationconcentrated
  7. custom176.1 (MH+), 0.32 min.