反应详情

To a room temperature suspension of 6.72 g of product from Example 114 in 200 ml methylene chloride is added, dropwise over 15 minutes, 10.05 g of product from Example 99 dissolved in 160 ml of methylene chloride. The reaction is stirred at room temperature for 10 minutes, followed by the dropwise addition of 12.73 g of triethylamine. The solution is stirred at room temperature for 19 hours, poured into a solution consisting of equal volumes saturated sodium bicarbonate, saturated sodium chloride and water, and extracted with 50/50 chloroform/methylene chloride. The organic layers are washed with saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel: 25% ethyl acetate/hexane) to give 10.75 g of the desired product as pale yellow crystals.

1. additionis added, dropwise over 15 minutes
2. stirringThe solution is stirred at room temperature for 19 hours
3. additionpoured into a solution
4. extractionextracted with 50/50 chloroform/methylene chloride
5. washThe organic layers are washed with saturated sodium chloride
6. customdried
7. concentrationconcentrated in vacuo
8. customThe residue is purified by column chromatography (silica gel: 25% ethyl acetate/hexane)