反应详情

温度

90 °C

A solution of the product from step (ii) (0.174 g) and sodium hydride (60% wt. disp. oil, 0.039 g) in DMF (10 ml) was stirred at 50° C. for 1 hour. The product from example 3 step (vi)-(vii) (0.200 g) was added and the mixture was refluxed at 90° C. for 3 hours. The mixture was partitioned between 2M sodium hydroxide and diethyl ether. The aqueous layer was acidified with 2M hydrochloric acid, extracted with ethyl acetate and the organic layer dried and concentrated under reduced pressure to give an oil. The residue was purified using RP prep HPLC. Yield 0.061 g

1. customThe mixture was partitioned between 2M sodium hydroxide and diethyl ether
2. extractionextracted with ethyl acetate
3. customthe organic layer dried
4. concentrationconcentrated under reduced pressure
5. customto give an oil
6. customThe residue was purified