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

HRID 1729313
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HRID 1729313 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27603511-(3-Phenoxypropyl)piperazineHCID 3015589Uracil, 6-chloro-1-methyl-

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-7398bf8ce5ba4f0196340b40394907b1
출처 데이터셋
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05332739

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