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Toluene → 1-(2,6-Dimethoxy-4-pyridyl)piperazine

HRID 333955
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HRID 333955 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7](Cl)[CH:6]=[C:5]([O:10][CH3:11])[N:4]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C1(C)C=CC=CC=1>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:6]=[C:5]([O:10][CH3:11])[N:4]=1
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참가 물질

5

반응물 3

HCID 1140TolueneHCID 4837PiperazineHCID 123244194-Chloro-2,6-dimethoxypyridine

생성물 1

HCID 668358261-(2,6-Dimethoxy-4-pyridyl)piperazine

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2.5 g (13 mmol) 2,6-dimethoxy-4-chloro-pyridine and 6.21 g (65 mmol) piperazine were heated at reflux in 22 ml anhydrous pyridine for 20 hours. After cooling (precipitation was detected) 50 ml of toluene was added and the suspension was filtered. The filtrate was concentrated under reduced pressure, piperazine and pyridine were azeotropically removed by repeated evaporation with toluene (five times). The residue was triturated with diethylether/petrolether (1:1) and dried in vacuo. The product was obtained as yellow solid and used directly in the next step.

후처리

  1. additionwas added
  2. filtrationthe suspension was filtered
  3. concentrationThe filtrate was concentrated under reduced pressure, piperazine and pyridine
  4. customwere azeotropically removed
  5. customevaporation with toluene (five times)
  6. customThe residue was triturated with diethylether/petrolether (1:1)
  7. customdried in vacuo
  8. customThe product was obtained as yellow solid

출처 및 근거

ORD 기록
ord-e9e29214697d4a22b51c7767628b2b4e
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08883791B2

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