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1-Butanol → 1-Piperazinebutanenitrile, 4-(2-pyrimidinyl)-

HRID 745209
ノート
印刷プレビュー

反応式

HRID 745209 の反応式
Cl[CH2:2][CH2:3][CH2:4][C:5]#[N:6].[N:7]1[CH:12]=[CH:11][CH:10]=[N:9][C:8]=1[N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.C(=O)([O-])[O-].[Na+].[Na+].C(O)CCC>O>[C:5]([CH2:4][CH2:3][CH2:2][N:16]1[CH2:17][CH2:18][N:13]([C:8]2[N:9]=[CH:10][CH:11]=[CH:12][N:7]=2)[CH2:14][CH2:15]1)#[N:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 2631-ButanolHCID 10340Sodium CarbonateHCID 123364-ChlorobutyronitrileHCID 887471-(2-Pyrimidinyl)piperazine

生成物 1

HCID 3986541-Piperazinebutanenitrile, 4-(2-pyrimidinyl)-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 4-chlorobutyronitrile (3.3 g; 0.032 mol), 1-(2-pyrimidinyl)piperazine (3.3 g; 0.032 mol), sodium carbonate (6.4 g; 0.0608 mol) and n-butanol (50 ml) was heated under reflux for 19 hours. After completion of the reaction, the resultant mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by silica gel chromatography to give 1-(3-cyanopropyl)-4-(2-pyrimidinyl)-piperazine. M.P., 56°-57° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 19 hours
  3. customAfter completion of the reaction
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with a saturated sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customthe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-6648ebb3fd8e4c8099da983c5c0a5785
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04598078

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート