Piperazine → 1-(4,6-Dimethylpyridin-2-YL)piperazine

HRID 880469ノート

反応式

HRID 880469 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:8]1[CH:13]=[C:12]([CH3:14])[CH:11]=[C:10]([CH3:15])[N:9]=1>COCCOCCOC.[Cl-].[Na+].O>[CH3:14][C:12]1[CH:11]=[C:10]([CH3:15])[N:9]=[C:8]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[CH:13]=1

参加物

5

反応物 2

HCID 4837PiperazineHCID 125083782-Chloro-4,6-dimethylpyridine

生成物 1

HCID 233680631-(4,6-Dimethylpyridin-2-YL)piperazine収率 92.4%

試薬・触媒・溶媒 2

HCID 8150Diglyme溶媒2 回HCID 57417360Sodium chloride; water溶媒

実験手順

A solution of piperazine (195 g, 2.26 mol) in diglyme (250 mL) was heated to 160° C. and a solution of 2-chloro-4,6-dimethylpyridine (40 g, 0.283 mol) in diglyme (150 mL) was added over a period of 30 min. The mixture was maintained at this temperature for 36 hand then the reaction mixture was allowed to cool to ambient temperature, diluted with brine and extracted with ethyl acetate (3×500 mL). The combined organic layers were washed with brine (2×100 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to give the crude compound. Vacuum distillation to remove diglyme afforded 1-(4,6-dimethyl-2-pyridyl)piperazine (50 g, 92%) as an oil.

後処理

  1. temperatureThe mixture was maintained at this temperature for 36 hand
  2. extractionextracted with ethyl acetate (3×500 mL)
  3. washThe combined organic layers were washed with brine (2×100 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give the crude compound
  7. distillationVacuum distillation
  8. customto remove diglyme

出典と根拠

ORDレコード
ord-db10b6d3cbbd4a678c3bfb0ef46b2db1
出典データセット
uspto-grants-2015_03
特許番号
US08993574B2

反応ノート

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