تفاعل #433859

ord-b672429898944e23b01a2d853ad34746

معادلة التفاعل

Sc1ccc2cc(Br)ccc2c1
6-bromonaphthalene-2-thiol
N#Cc1ccc(F)cc1C(F)(F)F
4-fluoro-2-trifluoromethyl benzonitrile
CCN(CC)CC
triethylamine
N#Cc1ccc(Sc2ccc3cc(Br)ccc3c2)cc1C(F)(F)F
4-(6-bromonaphth-2-ylthio)-2-trifluoromethylbenzonitrile

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed with water (3×25 ml) and brine (25 ml)
  2. 2
    تجفيفdried (MgSO4)
  3. 3
    أخرىevaporated
  4. 4
    أخرىto give a yellow oil
  5. 5
    أخرىCrystallisation from methanol (20 ml)

الإجراء التجريبي

A mixture of 6-bromonaphthalene-2-thiol (956 mg) and 4-fluoro-2-trifluoromethyl benzonitrile (756 mg) in dimethylformamide (15 ml), at ambient temperature, was treated dropwise with triethylamine (504 mg). After stirring at ambient temperature for 3 hours the reaction mixture was diluted with ethyl acetate (100 ml), washed with water (3×25 ml) and brine (25 ml), dried (MgSO4) and evaporated to give a yellow oil. Crystallisation from methanol (20 ml) gave 4-(6-bromonaphth-2-ylthio)-2-trifluoromethylbenzonitrile (1.176 g, mp 114-116° C.;

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07173025B1uspto-grants-2007_02