[N:1]([O-:3])=O.[Na+].[CH2:5]([N:9]([CH2:16][CH2:17][CH2:18][CH3:19])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH2:6][CH2:7][CH3:8].Cl.[OH-].[Na+]>O>[CH2:5]([N:9]([CH2:16][CH2:17][CH2:18][CH3:19])[C:10]1[CH:15]=[CH:14][C:13]([N:1]=[O:3])=[CH:12][CH:11]=1)[CH2:6][CH2:7][CH3:8]A solution was prepared by dissolving 18.5 g (0.26 mol) of sodium nitrite, of a purity of 97%, in 30 ml of water. This solution was added dropwise to a solution composed of 51.3 g (0.25 mol) of N,N-dibutylaniline, 200 g of water and 105 ml of conc HCl (35 to 38%) at a temperature between 10° and 20° C. for one-half hour. After stirring the solution obtained for one hour, the solution was neutralized to pH 8 with a 15% aqueous solution of sodium hydroxide. The crystals obtained were filtered, washed sufficiently on filter paper and thereafter dried with hot-air at 50° C. for 48 hours. 28.1 g of N,N-dibutyl-p-nitrosoaniline with a melting point of 122°~124° C. was obtained. The yield was 48.0%.
불러오는 중…
