Reference of 112970-44-2, A common heterocyclic compound, 112970-44-2, name is 2-Bromo-3-methoxyaniline, molecular formula is C7H8BrNO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A solution of Intermediate iSA (3.25 g, 16.09 mmol) and potassium 0-ethyl carbonodithioate (6.45 g, 40.2 mmol) in DMF (20 mL) was heated at 135 C under argon for 6.0 h. HPLC and LCMS indicated a completion of the reaction. The mixture was cooled to room temperature, diluted with 20 mL water, followed by addition of 30 mL 1.0 N HC1. The precipitate formed was collected by filtration, washed with water, dried under vacuum and then chased with toluene (3X) to yield Intermediate 15B (3.1 g, 15.71 mmol, 98 % yield) as a brown solid. It was used for the next step without further purification. ?H NMR (500MHz, DMSO-d6) 13.77 (br. s., 1H), 7.38 (t, J=8.1 Hz, 1H), 6.94 (t, J=8.1 Hz, 2H), 3.91 (s, 3H); LC-MS: method A, RT = 1.63 mm, MS (ESI) m/z:198.0(M+H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.