反应详情

温度

35 °C

4-(4-Methylsulfamoyl-4,7-diaza-spiro[2.5]oct-7-yl)-pyrrolo[2,3-d]pyrimidine-7-carboxylic acid tert-butyl ester (intermediate 4) (0.71 mmol) was dissolved in dry DMF (0.5 mL) and added Cs2CO3 (0.85 mmol) and (3-bromo-propyl)-benzene (0.085 mmol). Stirred at 35° C. for 1.5 h and then added H2O (2 mL). Extracted with EtOAc (3×2 mL) and the combined organic phases were concentrated in vacuo. The residual oil was treated with TFA (2 mL) at rt→45° C. for 1.5 h. The crude reaction mixture was concentrated in vacuo and redissolved in DMSO (0.5 mL). The pure compounds were obtained by standard preparative HPLC purification of the reaction mixture.

1. extractionExtracted with EtOAc (3×2 mL)
2. concentrationthe combined organic phases were concentrated in vacuo
3. additionThe residual oil was treated with TFA (2 mL) at rt→45° C. for 1.5 h
4. customThe crude reaction mixture
5. concentrationwas concentrated in vacuo
6. dissolutionredissolved in DMSO (0.5 mL)
7. customThe pure compounds were obtained by standard preparative HPLC purification of the reaction mixture