تفاعل #2186210

ord-1c25976a6a2647f7af53a1dd9b8001a2

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled below 5° C
  2. 2
    استخلاصextracted with AcOEt after dilution with saline
  3. 3
    تجفيفThe organic phase is dried over sodium sulfate
  4. 4
    أخرىevaporated
  5. 5
    أخرىthe residue column chromatographed (silica gel, AcOEt/EtOH 95:5)

الإجراء التجريبي

712 mg (4 mmol) 3-Piperazin-1-yl-phenol are dissolved in 30 mL DMF under argon and cooled below 5° C. After addition of 1.38 g (2.5 eq.) K2CO3, 166 mg (0.25 eq.) KI and 888 mg (1 eq.) 2-(3-bromo-propoxy)-tetrahydro-pyran, the suspension is stirred at room temperature for 20 hours, then extracted with AcOEt after dilution with saline. The organic phase is dried over sodium sulfate, evaporated and the residue column chromatographed (silica gel, AcOEt/EtOH 95:5) to yield 630 mg (48%) desired product as a light yellowish resin.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07569337B2uspto-grants-2009_08