HRID422551

反应详情

EQUATION

反应方程式

HRID 422551 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a 15-ml round-bottom flask were added 4-methyl-3-(1-methylphthalazin-6-yl)benzoic acid (51 mg, 183 μmol), hatu (105 mg, 275 μmol), ethylamine (2M solution in THF (275 μl, 550 μmol), and chloroform (1000 μl). 0.5 ml of N,N-Dimethylformamide was next added to the mixture, and the resulting golden yellow solution was stirred at RT for 3 h, during which LC-MS indicated completion of reaction. The reaction mixture was diluted with EtOAc and washed with water and brine, dried over MgSO4, filtered, and concentrated in vacuo. CombiFlash purification (1% to 5% MeOH/CH2Cl2) afforded the title compound (26) as a tan amorphous solid. MS (ES+): 306.2 (M+H)+.

WORKUP

后处理

  1. customcompletion of reaction
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customCombiFlash purification (1% to 5% MeOH/CH2Cl2)