N-Methyl-4-nitroaniline → N-Methyl-N-(4-nitrophenyl)phosphoramidic dichloride
반응식
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([NH:8][CH3:9])=[CH:6][CH:5]=1)([O-:3])=[O:2].[O:12]=[P:13](Cl)([Cl:15])[Cl:14]>C1(C)C=CC=CC=1>[CH3:9][N:8]([C:7]1[CH:10]=[CH:11][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)[P:13]([Cl:15])([Cl:14])=[O:12]참가 물질
4
실험 절차
p-Nitro-N-methylaniline (9.3 g, 0.061 mol) and 9 mL (0.1 mol) POCl3 were heated in 50 mL toluene to 90°-95° C. overnight. The solution was cooled and filtered. The volatiles were removed from the filtrate, giving 15.3 g of a purple, viscous oil. NMR (CDCl3): AA'XX' quartet from δ7.45-7.35 (4H), 3.37 (d,3H, J=14-15 Hz). No N--H was observed in the NMR. Due to an expected very high boiling point, this material was not distilled but used directly in the preparation of N-Methyl-N-(4-nitrophenyl) phosphoric triamide in the following Example VI.