HRID421795

反应详情

EQUATION

反应方程式

HRID 421795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 1-cyclobutylbutane-1,3-dione (69 mg, 0.49 mmol), N-[3-(trifluoromethyl)phenyl]urea (100 mg, 0.49 mmol) and 4-cyanobenzaldehyde (64.2 mg, 0.49 mmol) in tetrahydrofuran (250 ml) is added polyphosphoric acid ethyl ester (300 mg). The reaction mixture is stirred at reflux for 18 hours. After cooling to room temperature, the solvent is removed in vacuo and the crude product is purified by preparative HPLC (RP18 column; eluent: acetonitrile/0.1% aq. formic acid 10:90→90:10).

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. customthe solvent is removed in vacuo
  3. customthe crude product is purified by preparative HPLC (RP18 column; eluent: acetonitrile/0.1% aq. formic acid 10:90→90:10)