반응 #1118663

ord-6ac22737b2ca4d35bb5b4bd5a4110501

반응 방정식

C1CNCCN1
piperazine
COc1cccnc1Br
2-bromo-3-methoxypyridine
COc1cccnc1N1CCNCC1
1-(3-methoxy-2pyridinyl)piperazine
수율 82.0%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도Upon cooling
  2. 2
    추출extracted with CH2Cl2 (3×50 mL)
  3. 3
    기타The extracts were dried
  4. 4
    여과filtered
  5. 5
    농축concentrated under reduced pressure

실험 절차

Anhydrous piperazine (45.6 g) and 2-bromo-3-methoxypyridine (10.0 g) were heated neat in an autoclave at 100° C. for 20 h. Upon cooling, the mixture was treated with 5% NaCO3 (20 mL) and extracted with CH2Cl2 (3×50 mL). The extracts were dried using anhydrous K2CO3, filtered, and concentrated under reduced pressure to yield 1-(3-methoxy-2pyridinyl)piperazine (III; 8.43 g; 82%) after silica gel chromatography (CH2Cl2/MeOH/NH4OH; 93:7:0.7).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04954502uspto-grants-1990_09