تفاعل #356777

ord-660b33039c7649dcb4e5d398f7ec064a

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    أخرىthe two phases are separated
  3. 3
    غسيلThe organic phase is washed twice with distilled water and once with a saturated aqueous sodium chloride solution
  4. 4
    تجفيفThe organic phase is dried over sodium sulfate
  5. 5
    أخرىevaporated

الإجراء التجريبي

3.3 ml (35 mmol) of phosphorus tribromide are added dropwise to a solution of 35 g (103 mmol) of (2-benzyloxy-5-iodophenyl)methanol (Example 3A) in 350 ml of toluene at 40° C. The temperature of the reaction mixture is raised to 100° C. over the course of 15 min and the reaction mixture is stirred at this temperature for a further 10 min. After cooling, the two phases are separated. The organic phase is washed twice with distilled water and once with a saturated aqueous sodium chloride solution. The organic phase is dried over sodium sulfate and evaporated. The yield amounts to 41 g (99% of theory).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07446102B2uspto-grants-2008_11