反应详情

温度

100 °C

A mixture of 3.0 g of product from Example 95, 13.5 g of acetic anhydride, 0.081 g of 4-N,N-dimethylaminopyridine, 3.34 g of triethylamine and 25 ml of methylene chloride is heated, in a sealed tube, at 100° C. for 54 hours. The reaction is concentrated in vacuo, dissolved in methylene chloride, washed with saturated sodium bicarbonate, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel: 20% ethyl acetate/hexane) to give 1.42 g of the desired product as colorless crystals.

1. concentrationThe reaction is concentrated in vacuo
2. dissolutiondissolved in methylene chloride
3. washwashed with saturated sodium bicarbonate
4. customdried
5. concentrationconcentrated in vacuo
6. customThe residue is purified by column chromatography (silica gel: 20% ethyl acetate/hexane)