تفاعل #4076

ord-012a6b5e67c444bc94d607afb69c77fd

معادلة التفاعل

O=Nc1ccc(Nc2ccccc2)cc1
N-phenyl-4-nitrosoaniline
CCCCCCO
n-hexanol
[Na+].[OH-]
NaOH
Nc1ccc(Nc2ccccc2)cc1
N-phenyl-p-phenylenediamine

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04723040uspto-grants-1988_02