Methylurea → HCID 59828850, compound

Participants

Reaction Steps

Dissolve 4-cyanophenacyl bromide (10 g, 44.6 mmol) and methylurea (6.5 g, 89.3 mmol) in DMF (125 mL). Stir the reaction at 90° C. for 16 h under a nitrogen atmosphere. Cool to room temperature, dilute with hexane/EtOAc (1:1, 250 mL) and wash with 10% aqueous NaCl (4×75 mL). Collect the organic phase, concentrate in vacuo and purify the crude mixture by chromatography on silica gel (330 g) eluting with DCM/methanol (1:0 to 24:1 gradient) to obtain the desired intermediate (2.3 g, 26%). MS (ES+) m/z: 200.2 (M+H)+.

Provenance & Evidence