Methyl iodide → HCID 68295953, compound

Participants

Reaction Steps

4-(4-Phenethylsulfamoyl-4,7-diaza-spiro[2.5]oct-7-yl)-pyrrolo[2,3-d]pyrimidine-7-carboxylic acid tert-butyl ester (intermediate 6) (0.78 mmol) was dissolved in dry DMF (5 mL) and added K2CO3 (1.56 mmol) and iodomethane (1.17 mmol). Stirred at rt for 3 h and then added H2O (20 mL). Extracted with EtOAc (3×20 mL) and the combined organic phases were concentrated in vacuo. Purified by flash chromatography on silica using EtOAc in heptane as eluent. The obtained compound was treated with TFA (2 mL) at rt for 1.5 h. The crude reaction mixture was added sat. Na2CO3 to pH=7 and the extracted with EtOAc (3×10 mL). The combined organic phases was washes with brine (10 mL), dried (Na2SO4), filtered and concentrated in vacuo. The pure compound was obtained by flash chromatography on silica using EtOAc in heptane as eluent.

Provenance & Evidence