Methyl iodide → HCID 23654624, compound

Participants

Reaction Steps

A mixture of 3,4-dibromo-2-methoxy-5-methyl-6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepine (32.5 mg, 9.30 μmol), MeI (5.8 μl, 93.0 μmol), Na2CO3 (19.7 mg, 18.3 μmol) and DMF (5 ml) was stirred for 3 d at room temperature. The reaction was quenched with sat. aq. NaHCO3 and extracted with EtOAc. The organic layer was dried over Na2SO4, concentrated in vacuo and purified by column chromatography to give 19.0 mg (56%) of 3,4-dibromo-2-methoxy-5,7-dimethyl-6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepine. 1H-NMR (CDCl3) δ 3.89 (s, 3H), 3.63 (m, 1H), 3.25 (m, 1H), 2.88 (m, 3H), 2.30 (s, 3H), 2.28 (dd, 1H), 2.14 (m, 1H), 1.26 (d, 3H) ppm.

Provenance & Evidence