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

HRID 1729313
ノート
印刷プレビュー

反応式

HRID 1729313 の反応式
[C:1]1([O:7][CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:18]1[N:23]([CH3:24])[C:22](=[O:25])[NH:21][C:20](=[O:26])[CH:19]=1.C(N(CC)CC)C>C(O)(C)C>[CH3:24][N:23]1[C:18]([N:14]2[CH2:15][CH2:16][N:11]([CH2:10][CH2:9][CH2:8][O:7][C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:12][CH2:13]2)=[CH:19][C:20](=[O:26])[NH:21][C:22]1=[O:25]
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 27603511-(3-Phenoxypropyl)piperazineHCID 3015589Uracil, 6-chloro-1-methyl-

生成物 1

HCID 190118701-methyl-6-[4-(3-phenoxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione収率 68.1%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

1.3 g of 1-(3-phenyloxypropyl)piperazine and 0.5 g of 6-chloro-1-methyl-2,4(1H,3H)-pyrimidinedione were dissolved in 15 ml of isopropanol, and 2.7 ml of triethylamine was then added. Next, the solution was heated under reflux with stirring for 12 hours and then allowed to stand for cooling, and the solvent was distilled off. The resultant residue was dissolved in 100 ml of chloroform. The chloroform layer was washed with water, dried over anhydrous sodium sulfate and then concentrated under reduced pressure to obtain an oily product. This oily product was purified through a silica gel column chromatograph (chloroform/methanol=30/1 in volume ratio), thereby obtaining 0.73 g of 1-methyl-6-[4-(3-phenoxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione.

後処理

  1. temperatureNext, the solution was heated
  2. temperatureunder reflux
  3. temperaturefor cooling
  4. distillationthe solvent was distilled off
  5. dissolutionThe resultant residue was dissolved in 100 ml of chloroform
  6. washThe chloroform layer was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customto obtain an oily product
  10. customThis oily product was purified through a silica gel column chromatograph (chloroform/methanol=30/1 in volume ratio)

出典と根拠

ORDレコード
ord-7398bf8ce5ba4f0196340b40394907b1
出典データセット
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05332739

反応ノート

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