Methylamine → HCID 54146006, compound

Participants

Reaction Steps

At 0° C., 51 g of N-tert-butyl-5-bromomethyl-2-methanesulfonylbenzenesulfonamide (55% by weight A 28.05 g=0.669 mol) dissolved in 250 ml of THF are added to a solution of 59.5 ml (0.69 mol) of a 40% strength aqueous methylamine solution in 150 ml of THF. Stirring is continued at 0-5° C. for 2-3 h. For work-up, the solution is completely concentrated, the residue is taken up in plenty of 2N HCl and extracted with diethyl ether (2×200 ml). The acidic aqueous phase is adjusted to pH 9 with 4N NaOH and extracted with ethyl acetate (3×200 ml). The combined ethyl acetate extracts are washed with water, dried over Na2SO4 and evaporated in vacuo. 17 g (73.7%) of N-tert-butyl-5-methylaminomethyl-2-methanesulfonylbenzenesulfonamide of melting point 76-78° C. are obtained as residue.

Provenance & Evidence