反应详情

温度

60 °C

The compound of step 2 (50 mg, 0.14 mmol)) was dissolved in DMF (3 ml) and sodium hydride (60% dispersion in mineral oil, 6.2 mg, 0.15 mmol) was added followed by 1-bromomethyl-3-methyl-benzene (27 mg, 0.14 mmol). The mixture was stirred overnight. Then lithium hydroxide (1 M solution in water, 0.42 ml) and dioxane (1 ml) were added and the mixture heated to 60° C. for 1 h. The residue was partitioned between 2 N hydrochloric acid and EA and the aqueous phase was extracted with EA. The combined organic phases were dried over sodium sulfate and evaporated to dryness. The residue was purified by RP HPLC (water/ACN gradient) to yield 5 mg of the title compound.

1. customThe residue was partitioned between 2 N hydrochloric acid and EA
2. extractionthe aqueous phase was extracted with EA
3. dry with materialThe combined organic phases were dried over sodium sulfate
4. customevaporated to dryness
5. customThe residue was purified by RP HPLC (water/ACN gradient)