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HCID 13105519, Verbindung → 1-(2-(Piperazin-1-YL)ethyl)-1,3-dihydro-2H-benzo[D]imidazol-2-one

HRID 354962
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 354962
C1(C[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][N:16]3[C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=4[NH:18][C:17]3=[O:25])[CH2:10][CH2:9]2)C=CC=CC=1.[H][H]>[Pd].CO>[N:11]1([CH2:14][CH2:15][N:16]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[NH:18][C:17]2=[O:25])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
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Komponenten

5

Edukt 2

HCID 13105519HCID 13105519, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 131056241-(2-(Piperazin-1-YL)ethyl)-1,3-dihydro-2H-benzo[D]imidazol-2-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 79 parts of 1,3-dihydro-1-{2-[4-(phenylmethyl)-1-piperazinyl]ethyl}-2H-benzimidazol-2-one and 320 parts of methanol is hydrogenated at normal pressure and at room temperature with 10 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The oily residue is alkalized with ammonium hydroxide and a small amount of water is added. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The oily residue solidifies on triturating in 4-methyl-2-pentanone. The product is filtered off and dried, yielding 1,3-dihydro-1-[2-(1-piperazinyl)ethyl]-2H-benzimidazol-2-one; mp. 122.6° C.

Aufarbeitung

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. additiona small amount of water is added
  4. extractionThe product is extracted with trichloromethane
  5. customThe extract is dried
  6. filtrationfiltered
  7. customevaporated
  8. customon triturating in 4-methyl-2-pentanone
  9. filtrationThe product is filtered off
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-25f7234205304057bd58fdcfe1b88913
Quelldatensatz
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04377578

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