Carbon Dioxide → HCID 66738888, compound

Participants

Reaction Steps

To the compound (R)—N,N-Diisopropyl-3-(2-benzyloxy-5-bromophenyl)-3-Phenylpropyl amine compound of formula (F) 25.8 Mg turnings, 400 ml THF, 0.87 g ethyl bromide and 3 crystal of iodine were added and reaction heated to 50° C. to 55° C. and further raised to 65° C. to 70° C. The reaction mass cooled to −60° C. to 70° C. and slowly added 200 g dry ice and stirred for 1 hour. Further the reaction temperature raised to −5° C. to 0° C. followed by slowly addition of 700 ml of 10% ammonium chloride solution. The reaction temperature raised to 25° C. to 35° C., maintained for 30 minutes and finally filtered and washed with 2×25 ml R.O. Water. Layers were separated and further aqueous layer was charged and cooled to 0° C. to 5° C. and adjusted pH at 1 to 2 using conc. Hydrochloric acid solution followed by addition 500 ml MDC. The reaction temperature was raised to 25° C. to 35° C. followed by separation of layers and MDC was distilled under vacuum below at 50° C. The reaction mass was cooled to 25° C. to 35° C. followed by addition of 50 ml of methanol+300 ml of diisopropylether and cooled to 0° C. to 5° C. and finally washed with 2×25 ml diisopropylether to afford the title compound (R)-4-benzyloxy-3-(3-diisopropylamino-1-phenylpropyl)-benzoic acid hydrochloride of formula (G).

Provenance & Evidence