Triethylamine → HCID 9823946、化合物

HRID 1729289ノート

反応式

HRID 1729289 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 9823946HCID 9823946、化合物収率 86.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e3b52a76561d41cd97afe2cec71b36c4
出典データセット
uspto-grants-1994_07
特許番号
US05332739

反応ノート

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