تفاعل #2350732

ord-0475d82133434ba6ace8798478fd579e

المذيبات

ظروف التفاعل

درجة الحرارة
-78°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction mixture is warmed to room temperature
  2. 2
    استخلاصfollowed by extraction with tert-butyl methyl ether (3×)
  3. 3
    تجفيفThe combined organic layers are dried over sodium sulphate
  4. 4
    ترشيحfiltered
  5. 5
    تركيزconcentrated

الإجراء التجريبي

2 mmol of 2,6-diiodo-3-methoxy-4-(4-methoxy-butyl)-pyridine are added to a solution of 4 mmol n-butyllithium in 1.6 ml hexane and 10 ml tetrahydrofuran at −78° C. under an argon atmosphere. The reaction mixture is stirred at −78° C. for 15 minutes. 2 mmol of water are introduced and the reaction mixture is warmed to room temperature. 10% Aqueous ammonium chloride solution is added to the mixture followed by extraction with tert-butyl methyl ether (3×). The combined organic layers are dried over sodium sulphate, filtered and concentrated. The title compound is obtained from the residue by means of flash chromatography (SiO2 60 F) and identified based on its Rf value.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07851634B2uspto-grants-2010_12