反应详情

A mixture of 1C (6.83 g, 25 mmol), 3,4,5-trimethoxytoluene (4.56 g; 25 mmol), P2O5 (15.0 g) and dichloromethane (100 ml) is stirred at room temperature for 16 hours. Subsequently, the dichloromethane is distilled off and the residue is diluted with water and ethyl acetate. The organic phase is washed with water and concentrated. The residue is purified by preparative HPLC with acetonitrile:water 9:1 as eluent yielding the pure product as a yellow oil, 1.1 g, (10.1%).

1. distillationSubsequently, the dichloromethane is distilled off
2. additionthe residue is diluted with water and ethyl acetate
3. washThe organic phase is washed with water
4. concentrationconcentrated
5. customThe residue is purified by preparative HPLC with acetonitrile:water 9:1 as eluent