تفاعل #168911

ord-7688e123175b4b188dd13bf560e6eeec

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe whole was stirred at room temperature for 1 hour
  2. 2
    أخرىAll of the volatiles were removed in vacuo
  3. 3
    أخرىchromatographed on silica gel

الإجراء التجريبي

To a stirred mixture of tetrabromomethane (370 mg, 1.12 mmol) and triphenylphosphine (293 mg, 1.12 mmol) in dichloromethane (10 mL), was added (3-(2-(4-morpholinophenylamino)pyrimidin-4-ylthio)phenyl)methanol (400 mg, 1.01 mmol) portionwise. After being stirred at room temperature for 1 hour, another batch of tetrabromomethane (370 mg, 1.12 mmol) and triphenylphosphine (293 mg, 1.12 mmol) was added to the mixture and the whole was stirred at room temperature for 1 hour. All of the volatiles were removed in vacuo, and the residue was flash chromatographed on silica gel using ethyl acetate:dichloromethane (0:100→10:90) as eluant to give the product (208 mg, 45%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08846704B2uspto-grants-2014_09