HRID1471674

反应详情

EQUATION

反应方程式

HRID 1471674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 4-(2-(methylcarbamoyl)benzofuran-4-yl)piperazine-1-carboxylate (5.8 g, 16.1 mmol) was stirred in dichloromethane (50 mL) and trifluoroacetic acid (12.4 mL, 161.4 mmol) at rt for 4 h. The solvent was removed by rotary evaporation. The residue was dissolved in dichloromethane and 20 mL of 7 N NH3 in methanol was added. The mixture was evaporated onto silica gel, which was added to a silica gel column and eluted with 0-10% methanol (7 N NH3) in dichloromethane. The collected fractions were combined and the solvent was removed by rotary evaporation to give the title compound. Yield: 3.66 g, 87%. MS m/z 260.6 [M+H]+.

WORKUP

后处理

  1. customThe solvent was removed by rotary evaporation
  2. dissolutionThe residue was dissolved in dichloromethane
  3. addition20 mL of 7 N NH3 in methanol was added
  4. customThe mixture was evaporated onto silica gel, which
  5. additionwas added to a silica gel column
  6. washeluted with 0-10% methanol (7 N NH3) in dichloromethane
  7. customthe solvent was removed by rotary evaporation