Triethylamine → HCID 68526018, compound

Participants

Reaction Steps

To a stirred solution of 5-[(2-methyl-5-nitro-phenylamino)-methyl]-2-methylsulfanyl-pyrimidin-4-ylamine (112 mg, 0.37 mmol) and triethylamine (112 μL, 0.80 mmol) in THF (5 mL) is added a solution of triphosgene (38 mg, 0.13 mmol) in THF (1 mL) at 0° C., and the mixture is stirred for 3 hours at room temperature. The reaction mixture is diluted with EtOAc (10 mL), and washed with saturated aqueous sodium bicarbonate solution. The organic layer is dried over MgSO4, concentrated under reduced pressure and recrystallized from dichloromethane to give 3-(2-methyl-5-nitro-phenyl)-7-methylsulfanyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one (94 mg, 76%) as a white crystalline solid.

Provenance & Evidence