反应详情

温度

50 °C

An amount of 305 mg (0.99 mmol) of the compound from Example 19A and 355 mg (1.09 mmol) of caesium carbonate were suspended in 10 ml of acetone and admixed with 227 mg (0.99 mmol) of methyl 4-(bromomethyl)benzoate. The mixture was stirred at 50° C. for 3 h. The suspension was diluted with water. It was extracted with twice 15 ml of ethyl acetate. The combined organic phases were dried over sodium sulphate and freed from the solvent on a rotary evaporator. Purification by flash chromatography over silica gel with elution with cyclohexane/ethyl acetate (gradient 10:1→2:1) gave 284 mg (63% of theory) of the target compound.

1. extractionIt was extracted with twice 15 ml of ethyl acetate
2. dry with materialThe combined organic phases were dried over sodium sulphate
3. customfreed from the solvent on a rotary evaporator
4. customPurification by flash chromatography over silica gel
5. washwith elution with cyclohexane/ethyl acetate (gradient 10:1→2:1)
6. customgave 284 mg (63% of theory) of the target compound