HRID1471674
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was removed by rotary evaporation
- dissolutionThe residue was dissolved in dichloromethane
- addition20 mL of 7 N NH3 in methanol was added
- customThe mixture was evaporated onto silica gel, which
- additionwas added to a silica gel column
- washeluted with 0-10% methanol (7 N NH3) in dichloromethane
- customthe solvent was removed by rotary evaporation