反应详情

温度

40 °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) (0.047 mmol) was dissolved in dry DMF (0.5 mL) and added Cs2CO3 (0.071 mmol) and chloro-acetic acid methyl ester (0.071 mmol). Stirred at 40° C. for 2 h and then added H2O (1.5 mL). Extracted with EtOAc (3×1 mL) and the combined organic phases were washed with brine (1 mL) and concentrated in vacuo. The residual oil was treated with TFA (1 mL) at rt for 1 h. The crude reaction mixture was concentrated in vacuo and redissolved in DMSO (0.5 mL). The pure compound was obtained by standard preparative HPLC purification of the reaction mixture.

1. extractionExtracted with EtOAc (3×1 mL)
2. washthe combined organic phases were washed with brine (1 mL)
3. concentrationconcentrated in vacuo
4. additionThe residual oil was treated with TFA (1 mL) at rt for 1 h
5. customThe crude reaction mixture
6. concentrationwas concentrated in vacuo
7. dissolutionredissolved in DMSO (0.5 mL)
8. customThe pure compound was obtained by standard preparative HPLC purification of the reaction mixture