반응 #4076

반응 방정식

N-phenyl-4-nitrosoaniline

n-hexanol

NaOH

→

N-phenyl-p-phenylenediamine

반응 조건

후처리

1. 1
   기타To a 1-liter three-necked round bottom flask fitted with a stirrer, a condenser
2. 2
   온도heating
3. 3
   workup.WAITAfter another 15 minutes
4. 4
   기타returned to 100° C
5. 5
   workup.STIRRINGStirring
6. 6
   workup.WAITwas continued for one hour
7. 7
   온도while maintaining the reaction mixture at 100°-105° C

실험 절차

To a 1-liter three-necked round bottom flask fitted with a stirrer, a condenser and a thermometer were added 99.0 (0.5 mole) N-phenyl-4-nitrosoaniline, 254 g n-hexanol and 40 g (0.5 mole) aqueous NaOH (50% by weight). The dark reddish brown solution was stirred, heated to 100° C., at which point an exotherm developed, and heating was discontinued. A temperature rise to 120° C. was observed within 15 minutes. After another 15 minutes, the temperature returned to 100° C. Stirring was continued for one hour while maintaining the reaction mixture at 100°-105° C. Thereafter, a sample of the reaction mixture was analyzed by HPLC; no nitroso starting material was detected.

출처