تفاعل #1287384

ord-5dddb103589f4fae8d34157fdb9f3ffe

المذيبات

ظروف التفاعل

درجة الحرارة
38°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىIn a 100-ml flask fitted with a stirrer
  2. 2
    workup.ADDITIONTo this is added at 25° C
  3. 3
    أخرىcrystallized as a granular precipitate
  4. 4
    درجة الحرارةThe mixture is cooled to 0° C.
  5. 5
    workup.STIRRINGThe mixture is stirred at -2° C. for 1 hour

الإجراء التجريبي

In a 100-ml flask fitted with a stirrer and thermometer, 15.0 grams (0.06 mole) of 4-tert-octyl-2-nitroaniline is suspended in 20 ml of toluene. To this is added at 25° C. 17.3 grams (0.18 mole) of concentrated hydrochloric acid. The suspension is stirred at 38° C. for 1 hour followed by the addition of 6 ml of water. The mixture becomes thick as the corresponding hydrochloride salt crystallized as a granular precipitate. The mixture is cooled to 0° C. and diazotized by the addition over a period of 30 minutes of 4.3 grams (0.062 mole) of sodium nitrite in 6 ml of water keeping the temperature at -5° C. to -2° C. The mixture is stirred at -2° C. for 1 hour. Two phases occur. The combined phases contain the desired diazonium chloride and are used as is.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04904712uspto-grants-1990_02