反应详情

温度

50 °C

300 mg (1.13 mmol) of the compound from Example 232A together with 1.10 g (3.38 mmol) of caesium carbonate are placed in 12 ml acetone and treated with 456 mg (3.38 mmol) of bromo-methylcyclopropane. This is stirred for 2 hrs at 50° C. The reaction mixture is then diluted with 10 ml each of ethyl acetate and water and acidified with 1 N hydrochloric acid. The phases are separated and the aqueous phase is once again extracted with 10 ml ethyl acetate. The combined organic phases are dried over sodium sulphate, filtered and concentrated in vacuo. Further purification is effected by preparative HPLC [Method 10]. 60 mg (17% of theory) of the target compound are thus obtained.

1. customThe phases are separated
2. extractionthe aqueous phase is once again extracted with 10 ml ethyl acetate
3. dry with materialThe combined organic phases are dried over sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customFurther purification
7. custom60 mg (17% of theory) of the target compound are thus obtained