تفاعل #4018

ord-17f6266b5d2e48cc810a4fc82883f5f9

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe solution was concentrated
  2. 2
    أخرىto remove excess ethanol
  3. 3
    استخلاصthe resulting material was extracted with ether (500 ml)
  4. 4
    استخلاصThe organic extract
  5. 5
    غسيلwas washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml)
  6. 6
    أخرىevaporated
  7. 7
    أخرىto obtain an amber colored oil, which
  8. 8
    أخرىcrystallized
  9. 9
    أخرىupon standing at room temperature

الإجراء التجريبي

To a solution of 2-amino-4-trifluoromethylthiophenol hydrochloride (30.0 g) in ethanol (125 ml) was added 2-chloro-1,1,1-triethoxyethane (31.0 g). The mixture was heated for 1 hour at 60° C. The solution was concentrated to remove excess ethanol and the resulting material was extracted with ether (500 ml). The organic extract was washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml), and then evaporated to obtain an amber colored oil, which crystallized upon standing at room temperature (28.9 g; m.p. 52° C).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04723010uspto-grants-1988_02