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Hydrochloric Acid → 1-Phenyl-3-(piperidin-4-yl)imidazolidin-2-one

HRID 614372
ノート
印刷プレビュー

反応式

HRID 614372 の反応式
C([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[CH2:18][CH2:17][N:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:15]2=[O:25])[CH2:10][CH2:9]1)C1C=CC=CC=1.O.Cl.[H][H]>CO.[Pd]>[NH:8]1[CH2:9][CH2:10][CH:11]([N:14]2[CH2:18][CH2:17][N:16]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)[C:15]2=[O:25])[CH2:12][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 155726681-(1-Benzylpiperidin-4-yl)-3-phenylimidazolidin-2-oneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 205401631-Phenyl-3-(piperidin-4-yl)imidazolidin-2-one収率 93.6%

試薬・触媒・溶媒 2

HCID 23938Palladium
触媒
HCID 887Methanol溶媒

実験手順

11.1 g of 1-(1-benzyl-4-piperidinyl)-3-phenyl-2-imidazolidinone are dissolved in 85 ml of methanol, 34 ml of water and 3.2 ml of hydrochloric acid (chemically pure), and, with the addition of 1.2 g of a 5% palladium on charcoal catalyst, hydrogenated at room temperature and under normal pressure. The calculated amount of hydrogen has been taken up after approx. 15 hours. The reaction mixture is filtered to remove the catalyst and concentrated in a water jet vacuum. The crystalline residue is treated with 2N sodium carbonate solution and extracted with chloroform. The combined chloroform extracts are dried over sodium sulphate and concentrated in a water jet vacuum to yield 7.6 g of 1-(4-piperidinyl)-3-phenyl-2-imidazolidinone as a colourless oil which crystallises on standing; melting point 123°-124° C.

後処理

  1. customhydrogenated at room temperature
  2. filtrationThe reaction mixture is filtered
  3. customto remove the catalyst
  4. concentrationconcentrated in a water jet vacuum
  5. additionThe crystalline residue is treated with 2N sodium carbonate solution
  6. extractionextracted with chloroform
  7. dry with materialThe combined chloroform extracts are dried over sodium sulphate
  8. concentrationconcentrated in a water jet vacuum

出典と根拠

ORDレコード
ord-dc91ae9a1a864f0ab12319d18cd38383
出典データセット
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04144344

反応ノート

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