Triethylamine → HCID 9823946, 화합물

HRID 1729289노트

반응식

HRID 1729289 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[CH:19]=[CH:18][C:12]([O:13][CH2:14][CH2:15][CH2:16]Br)=[CH:11][CH:10]=1.[CH3:20][N:21]1[C:26]([N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)=[CH:25][C:24](=[O:33])[N:23]([CH3:34])[C:22]1=[O:35]>C(O)C>[Cl:8][C:9]1[CH:19]=[CH:18][C:12]([O:13][CH2:14][CH2:15][CH2:16][N:30]2[CH2:31][CH2:32][N:27]([C:26]3[N:21]([CH3:20])[C:22](=[O:35])[N:23]([CH3:34])[C:24](=[O:33])[CH:25]=3)[CH2:28][CH2:29]2)=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2235341-(3-Bromopropoxy)-4-chlorobenzeneHCID 128168731,3-Dimethyl-6-(piperazin-1-yl)pyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 9823946HCID 9823946, 화합물수율 86.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3 ml of triethylamine was added to 10 ml of an ethanol solution containing 2.5 g of 3-(4-chlorophenoxy)propyl bromide and 1.3 g of 1,3-dimethyl-6-(1-piperazinyl)-2,4(1H,3H)-pyrimidinedione, and the solution was then heated under reflux for 3 hours. Afterward, the reaction solution was concentrated to dryness, and the resultant residue was dissolved in chloroform and then washed with water. The thus obtained chloroform solution was dried and then concentrated, and the residue was recrystallized from ethanol/hexane, thereby preparing 1.96 g (yield: 86%) of 6-[4-(3-[4-chlorophenoxy]propyl)piperazin-1-yl]-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione.

후처리

  1. temperaturethe solution was then heated
  2. temperatureunder reflux for 3 hours
  3. concentrationAfterward, the reaction solution was concentrated to dryness
  4. dissolutionthe resultant residue was dissolved in chloroform
  5. washwashed with water
  6. dry with materialThe thus obtained chloroform solution was dried
  7. concentrationconcentrated
  8. customthe residue was recrystallized from ethanol/hexane

출처 및 근거

ORD 기록
ord-e3b52a76561d41cd97afe2cec71b36c4
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05332739

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