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Triethylamine → 1,3-dimethyl-6-[4-(4-nitrobenzyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione

HRID 1085249
ノート
印刷プレビュー

反応式

HRID 1085249 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8]Br)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:12][N:13]1[C:18]([NH:19][CH2:20][CH2:21]CNC2C=CC([N+]([O-])=O)=CC=2)=[CH:17][C:16](=[O:33])[N:15]([CH3:34])[C:14]1=[O:35].[CH2:36]([N:38](CC)CC)[CH3:37]>C(O)(C)C>[CH3:12][N:13]1[C:18]([N:19]2[CH2:20][CH2:21][N:38]([CH2:8][C:7]3[CH:10]=[CH:11][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=3)[CH2:36][CH2:37]2)=[CH:17][C:16](=[O:33])[N:15]([CH3:34])[C:14]1=[O:35]
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 8471TriethylamineHCID 660114-Nitrobenzyl bromideHCID 200612441,3-dimethyl-6-[3-(4-nitroanilino)propylamino]-2,4-(1H,3H)-pyrimidinedione2 回

生成物 1

HCID 104736221,3-dimethyl-6-[4-(4-nitrobenzyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

First, 0.48 g of 4-nitrobenzyl bromide, 0.5 g of 1,3-dimethyl-6-(piperazin -1-yl)-2,4(1H,3H)-pyrimidinedione (compound 2) and 0.5 ml of triethylamine were suspended in 5 ml of isopropanol, and the resulting suspension was then heated under reflux for 8 hours. Afterward, the used solvent was removed from the resulting reaction mixture by distillation under reduced pressure, and the residue was dissolved in chloroform and was then washed with water. The washed organic layer was dried over anhydrous sodium sulfate. Furthermore, the dried organic layer was subjected to distillation under reduced pressure so as to remove the solvent therefrom, and the residue was then purified through a silica gel column chromatograph (chloroform/methanol=50/1 to 20/1 in terms of volume ratio) in order to obtain 0.88 g of 1,3-dimethyl-6-[4-(4-nitrobenzyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione.

後処理

  1. temperaturethe resulting suspension was then heated
  2. temperatureunder reflux for 8 hours
  3. customAfterward, the used solvent was removed from the resulting reaction mixture by distillation under reduced pressure
  4. dissolutionthe residue was dissolved in chloroform
  5. washwas then washed with water
  6. dry with materialThe washed organic layer was dried over anhydrous sodium sulfate
  7. distillationFurthermore, the dried organic layer was subjected to distillation under reduced pressure so as
  8. customto remove the solvent
  9. customthe residue was then purified through a silica gel column chromatograph (chloroform/methanol=50/1 to 20/1 in terms of volume ratio) in order

出典と根拠

ORDレコード
ord-744d1405421e4baca24789681da47d84
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05008267

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