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

HRID 614372
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HRID 614372 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 155726681-(1-Benzylpiperidin-4-yl)-3-phenylimidazolidin-2-oneHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium
촉매
HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dc91ae9a1a864f0ab12319d18cd38383
출처 데이터셋
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04144344

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