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

HRID 333955
ノート
印刷プレビュー

反応式

HRID 333955 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e9e29214697d4a22b51c7767628b2b4e
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883791B2

反応ノート

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