反应详情

The product from step (b) (38.7 g) was dissolved in 600 ml of 2,6-lutidine and 120 ml of 1.0M HCl in diethyl ether was then added. The reaction mixture was refluxed overnite, using a Dean Stark trap, then concentrated in vacuo. The residue was taken up in 5% NaHCO3 whereupon solidification took place. The solids were filtered and washed with ether to afford the desired product as a light brown solid (25.7 g), mp 170°-171° C. 1H NMR consistent with the proposed structure.

1. temperatureThe reaction mixture was refluxed overnite
2. concentrationconcentrated in vacuo
3. filtrationThe solids were filtered
4. washwashed with ether