反应详情

The compound of step 1 (1.18 g, 4.12 mmol) and potassium carbonate (1.72 g, 12.4 mmol) were suspended in DMF (10 ml), m-cresol (450 mg, 4.12 mmol) was added, and the mixture was stirred at room temperature for 2 h. The volatiles were evaporated in vacuo, the residue was partitioned between EA and water, and the aqueous phase extracted with EA. The combined organic extracts were washed with a sodium chloride solution, dried over sodium sulfate, filtered and evaporated to dryness. The residue was purified by preparative RP HPLC (water/ACN gradient) to give 0.49 g of the title compound.

1. customThe volatiles were evaporated in vacuo
2. customthe residue was partitioned between EA and water
3. extractionthe aqueous phase extracted with EA
4. washThe combined organic extracts were washed with a sodium chloride solution
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customevaporated to dryness
8. customThe residue was purified by preparative RP HPLC (water/ACN gradient)