تفاعل #49740

ord-743f0184faad46bdaf8b57fb69cedb4f

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was warmed until reaction
  2. 2
    غسيلwashed with water, hydrochloric acid (2M), water
  3. 3
    تجفيفdried (MgSO4)
  4. 4
    ترشيحfiltered
  5. 5
    أخرىThe filtrate was evaporated to dryness
  6. 6
    workup.DISTILLATIONthe residue was distilled

الإجراء التجريبي

t-Butyl nitrite (3 ml) was added to a mixture of 3-amino-4-bromobenzotrifluoride (4 g) and dimethyl disulphide (15 ml) in chloroform. The mixture was warmed until reaction started when t-butyl nitrite (11 ml) and a solution of 3-amino-4-bromobenzotrifluoride (16 g) in chloroform were added simultaneously. The resultant mixture was stirred for 24 hours, washed with water, hydrochloric acid (2M), water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 4-bromo-3-(methylsulphenyl)benzotrifluoride (16.4 g) as a yellow oil, b.p. 84°-88° C. at 2 mm Hg.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05424276uspto-grants-1995_06