Trichloromethyl isocyanate → HCID 58203529, compound

Participants

Reaction Steps

Trichloro-isocyanato-methane (39 uL, 0.33 mmol, 2.0 eq) was added to 3-[3-(2-hydroxy-ethyl)-5-isopropyl-1-(4-methoxy-benzyl)-2,6-dioxo-1,2,3,6-tetrahydro-pyrimidine-4-carbonyl]-5-methyl-benzonitrile (76 mg, 0.165 mmol) in 2 mL of DCM. The reaction mixture was stirred at room temperature for 10 minutes. HPLC and LC-MS showed complete reaction of the starting materials. Ammonia gas was bubbled into 3 mL DCM in a test tube (keep bubbling for 5 minutes). The ammonia solution was added to the above reaction mixture. The reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was filtered and concentrated down and purified (silica gel, 0-80% EtOAC/hexane) to give a white powder (42 mg, 51%). LC-MS shows 505.0 (M+1).

Provenance & Evidence