تفاعل #348310

ord-fdf9225ee80143cc89f931117c9140e7

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added over a period of 20 minutes
  2. 2
    أخرىAfter half an hour of further reaction at 80°-90° C.
  3. 3
    أخرى(11/4 hours)
  4. 4
    أخرىwas then stripped to a temperature of 100° C. and 30 mm

الإجراء التجريبي

7.3 g of triethylenetetramine (0.05 mol) in 30 ml. of toluene was heated to 75° C. and a mixture of 5.3 g of sodium carbonate and 67.3 g of perfluorodecenyloxybenzene sulfonyl chloride was added over a period of 20 minutes while maintaining the temperature at 80° C. After half an hour of further reaction at 80°-90° C., the reaction mixture was stripped of solvent to a temperature of 150° C. and 45 mm mercury pressure. There was then added 16.4 g of behenic acid (0.05 mol) and 30 ml. of toluene and the mixture was reacted at 115°-120° C. until 0.05 mol of water had evolved (11/4 hours). The solvent was then stripped to a temperature of 100° C. and 30 mm. mercury pressure to yield the product, triethylenetetramine bis-(perfluorodecenyloxybenzene sulfonamide) monobehenamide, a tan, hard solid with good oil, water and soil repellancy.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04163754uspto-grants-1979_08