反应详情

温度

150 °C

A mixture of 0.88 g of product from Example 393, 5.0 ml of acetic anhydrideand 2.0 ml of lutidine is heated at 110°-115° C. for 2.5 hours, followed by increasing the temperature to 150° C. and then heated for 3 hours. The reaction mixture is diluted with ethyl acetate, washed 2 X with 1N hydrochloric acid, water, saturated sodium chloride, dried and concentrated in vacuo. The residue is dissolved in methylene chloride, filtered through a pad of hydrous magnesium silicate and reconcentrated in vacuo to give 0.569 g of the desired product.

1. temperatureis heated at 110°-115° C. for 2.5 hours
2. temperatureheated for 3 hours
3. washwashed 2 X with 1N hydrochloric acid, water, saturated sodium chloride
4. customdried
5. concentrationconcentrated in vacuo
6. dissolutionThe residue is dissolved in methylene chloride
7. filtrationfiltered through a pad of hydrous magnesium silicate