HRID1169695

反应详情

EQUATION

反应方程式

HRID 1169695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-amino-1-(2,4-dimethoxybenzyl)-4-(3-fluorophenyl)-6-methoxyquinolin-2-(1H)-one (62 mg, 0.143 mmol) in 3 mL of trifluoroacetic acid was added dimethyl sulfide (0.30 mL). After stirring for 2 days, the reaction was heated to reflux for 3 hours, then concentrated in vacuo. The crude residue was purified by flash chromatography through SiO2 (1-3% MeOH/CH2Cl2) to provide the titled product as a yellow solid. Proton NMR for the product was consistent with the titled compound. HRMS (ES) exact mass calculated for C16H13FN2O2 (M+H+): 285.1034. Found 285.1029.

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 3 hours
  3. concentrationconcentrated in vacuo
  4. customThe crude residue was purified by flash chromatography through SiO2 (1-3% MeOH/CH2Cl2)