反应详情

温度

110 °C

A mixture of 0.70 g of product from Example 88, 2.96 g of acetic anhydride, 0.027 g of 4-N,N-dimethylaminopyridine and 15 ml of pyridine is heated at 110° C. for 35 hours and at reflux temperature for 57 hours. The reaction is poured into water and extracted with methylene chloride. The organic layer is washed with saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel: 35% ethyl acetate/hexane) to give 0.366 g of product as light yellow crystals.

1. temperatureat reflux temperature for 57 hours
2. extractionextracted with methylene chloride
3. washThe organic layer is washed with saturated sodium chloride
4. customdried
5. concentrationconcentrated in vacuo
6. customThe residue is purified by column chromatography (silica gel: 35% ethyl acetate/hexane)