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Sodium Hydroxide → 2-(4-Benzylpiperazino)-6-ethyl-5-oxo-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine

HRID 569991
ノート
印刷プレビュー

反応式

HRID 569991 の反応式
S(O)(O)(=O)=O.[C:6]([N:9]1[CH2:14][CH2:13][N:12]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)(=[NH:8])[NH2:7].[OH-].[Na+].[CH2:24]([N:26]1[CH2:31][CH2:30][C:29](=O)[C:28](=[CH:33]OC)[C:27]1=[O:36])[CH3:25]>C(O)C>[CH2:15]([N:12]1[CH2:13][CH2:14][N:9]([C:6]2[N:7]=[CH:33][C:28]3[C:27](=[O:36])[N:26]([CH2:24][CH3:25])[CH2:31][CH2:30][C:29]=3[N:8]=2)[CH2:10][CH2:11]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
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 14798Sodium HydroxideHCID 27566524-Benzylpiperazine-1-carboxamidine hemisulfateHCID 540921521-Ethyl-3-methoxymethylenepiperidine-2,4-dione

生成物 1

HCID 137841212-(4-Benzylpiperazino)-6-ethyl-5-oxo-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine収率 80.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension which had been obtained by adding 1.56 g of 1-amidino-4-benzylpiperazine sulfate to an ethanol solution of 0.23 g of sodium hydroxide, 1.07 g of 1-ethyl-3-methoxymethylenepiperidine-2,4-dione (Referential Example 37) was added. The resultant mixture was refluxed for 2 hours. After distilling off ethanol, water was added to the residue, followed by extraction with chloroform. After drying the chloroform layer, it was concentrated to obtain 1.4 g of 2-(4-benzylpiperazino)-6-ethyl-5-oxo-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (yield: 69%).

後処理

  1. customTo a suspension which had been obtained
  2. additionwas added
  3. distillationAfter distilling off ethanol, water
  4. additionwas added to the residue
  5. extractionfollowed by extraction with chloroform
  6. dry with materialAfter drying the chloroform layer, it
  7. concentrationwas concentrated

出典と根拠

ORDレコード
ord-9801a83f8e1a42d89eafa66ceaa379e3
出典データセット
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04734418

反応ノート

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