Methylamine → HCID 16082, compound

Participants

Reaction Steps

A mixture of 2,4-dichloro-6-phenyl-1,3,5-triazine (16.0 g, 70.8 mmol, 1.00 equiv) dissolved in 1:1 CH3CN:H2O (80 mL) was cooled (0° C.), and a solution of NH2Me (8.00 g, 27.5% solution in H2O, 70.8 mmol, 1.00 equiv) was added. The pH of the reaction mixture was adjusted to 9-10 by treating with 1 N NaOH. The pH was maintained at 9-10 for 15 min (product formation monitored by LCMS). The mixture was diluted with water, and filtered to provide 12 g of crude product (filtered solid was washed with additional water). A portion of this material (8 g) was purified by HPLC to afford 3.6 g of the title compound. MS (ES+): m/e 221.1 [M+H]+.

Provenance & Evidence