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Piperazine → 1-[2-(1-Methylethylamino)-3-pyrazinyl]piperazine

HRID 1449709
ノート
印刷プレビュー

反応式

HRID 1449709 の反応式
Cl[C:2]1[C:7]([NH:8][CH:9]([CH3:11])[CH3:10])=[N:6][CH:5]=[CH:4][N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>C1(C)C(C)=CC=CC=1.Cl>[CH3:10][CH:9]([NH:8][C:7]1[C:2]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[N:3][CH:4]=[CH:5][N:6]=1)[CH3:11]
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 2

HCID 4837PiperazineHCID 214776373-Chloro-N-(propan-2-yl)pyrazin-2-amine

生成物 1

HCID 214776571-[2-(1-Methylethylamino)-3-pyrazinyl]piperazine

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 7237O-Xylene溶媒

実験手順

A solution of 2-chloro-3-(1-methylethylamino)pyrazine (PREPARATION 6, 1.6 g) and piperazine (4.3 g) in xylene (10 ml) is refluxed for 26 hr. The mixture is cooled to 0° and diluted with concentrated hydrochloric acid (8 ml). The xylene is decanted and ether is added and also decanted from the salts. The salts are diluted with excess aqueous sodium hydroxide (5%) and dichloromethane. The phases are separated. The aqueous phase is extracted three more times with dichloromethane. The combined organic extracts are dried over sodium sulfate and concentrated to give a liquid mixture which is flash chromatographed on silica gel eluting with methanol/chloroform (5/95). The appropriate fractions are pooled and concentrated to give the title compound, NMR (CDCl3) 1.27, 1.83, 3.04, 4.12, 4.78, 7.49 and 7.72 δ.

後処理

  1. temperatureThe mixture is cooled to 0°
  2. customThe xylene is decanted
  3. additionether is added
  4. customalso decanted from the salts
  5. additionThe salts are diluted with excess aqueous sodium hydroxide (5%) and dichloromethane
  6. customThe phases are separated
  7. extractionThe aqueous phase is extracted three more times with dichloromethane
  8. dry with materialThe combined organic extracts are dried over sodium sulfate
  9. concentrationconcentrated
  10. customto give a liquid mixture which
  11. customchromatographed on silica gel eluting with methanol/chloroform (5/95)
  12. concentrationconcentrated

出典と根拠

ORDレコード
ord-15d9914829f64caab789814b110946f3
出典データセット
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05599930

反応ノート

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