반응 #2186210

반응 방정식

3-Piperazin-1-yl-phenol

K2CO3

2-(3-bromo-propoxy)-tetrahydro-pyran

→

desired product

수율 49.4%

3-{4-[3-(Tetrahydro-pyran-2-yloxy)-propyl]-piperazin-1 -yl}-phenol

수율 49.4%

용매

DMF

반응 조건

후처리

1. 1
   온도cooled below 5° C
2. 2
   추출extracted with AcOEt after dilution with saline
3. 3
   건조The organic phase is dried over sodium sulfate
4. 4
   기타evaporated
5. 5
   기타the residue column chromatographed (silica gel, AcOEt/EtOH 95:5)

실험 절차

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.

출처