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

HRID 37860

反応式

HRID 37860 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[Cl-].[Na+]>COCCOCCOC.O>[CH3:8][C:6]1[CH:5]=[C:4]([CH3:9])[N:3]=[C:2]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[CH:7]=1

参加物

6

反応物 3

HCID 4837PiperazineHCID 5234Sodium ChlorideHCID 125083782-Chloro-4,6-dimethylpyridine2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8150Diglyme溶媒2 回

実験手順

A solution of 2-chloro-4,6-dimethylpyridine (30 g, 0.212 mol) in diglyme (100 mL) was added over 25-30 min. to a refluxing solution of anhydrous piperazine (147 g, 1.70 mol) in diglyme (150 mL). Heating was continued for 18 h (whereby TLC showed absence of 2-chloro-4,6-dimethylpyridine), then the mixture was cooled to room temperature and diluted with water (3 L). Sodium chloride (50 g) was added and the solution was extracted with ethyl acetate (300 mL×3); the combined extracts were washed with brine (200 mL), dried over anhydrous sodium sulfate and concentrated in vacuo (up to 110° C. & ˜15 mmHg; to remove maximum diglyme) to afford 1-(4,6-dimethyl-pyridin-2-yl)-piperazine (42 g, 103.3%, the G.C. spectrum showed 86.4% product, 10.7% diglyme, and 2.1% dimer.)

後処理

  1. temperatureHeating
  2. extractionthe solution was extracted with ethyl acetate (300 mL×3)
  3. washthe combined extracts were washed with brine (200 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo (up to 110° C.
  6. customto remove maximum diglyme)

出典と根拠

ORDレコード
ord-7c8f3e190dd045068e2064d3e4637ddc
出典データセット
uspto-grants-2013_09
特許番号
US08524705B2

関連ノート

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