Reaction #1444135
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05354772
Conditions: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: 562.9 g. (4.08 moles) of N-isopropylaniline is rapidly added to a solution of the crude product of Step 1 in 500 ml. of dimethylformamide stirred at 50° C. under nitrogen. The reaction mixture is stirred at 100° C. under nitrogen for 10 hours and allowed to cool to room temperature overnight. The reaction mixture is heated to 60° C., 2 l of water is added, and the mixture is cooled to 10° C. The obtained solids are collected, washed twice with 500 ml. portions of water and dissolved in 550 ml. of 95% ethanol at 75° C. The solution is cooled to 0° C., and the obtained solids are collected, washed three times with 100 ml. portions of 95% ethanol and vacuum dried at 35°-40° C. for 4 hours to obtain the 95.3% pure yellow product (466 g. (80.2% (two steps))), m.p. 78°- 81° C. to cool to room temperature overnight The reaction mixture is heated to 60° C. the mixture is cooled to 10° C The obtained solids are collected washed twice with 500 ml portions of water and dissolved in 550 ml at 75° C The solution is cooled to 0° C. the obtained solids are collected washed three times with 100 ml portions of 95% ethanol and vacuum dried at 35°-40° C. for 4 hours
Source ID: ord-6bd01cd2b12b4462a0e0eede11e20c82