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Hydrochloric Acid → 5-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride

HRID 1162328
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1162328
[CH3:1][C:2]1[N:6]2[C:7](=[O:24])[N:8]([CH2:10][CH:11]3[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]3)[CH2:9][C:5]2=[CH:4][N:3]=1.[ClH:25]>C(O)C>[ClH:25].[ClH:25].[CH3:1][C:2]1[N:6]2[C:7](=[O:24])[N:8]([CH2:10][CH:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[CH2:9][C:5]2=[CH:4][N:3]=1
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Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 23138425tert-butyl 4-((5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)methyl)-1-piperidinecarboxylate

Produkt 1

HCID 231381375-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochlorideAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To tert-butyl 4-((5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)methyl)-1-piperidinecarboxylate (3.5 g) obtained in Example 85a) was added concentrated hydrochloric acid (10 ml), and mixed for 10 minutes. To the reaction mixture was added ethanol, and the solvent was distilled off under reduced pressure. To the residue was further added ethanol, and the solvent was distilled off under reduced pressure. To the residue was added isopropyl alcohol, and the precipitate was collected by filtration. The precipitate was washed sequentially with isopropyl alcohol and diethyl ether and dried under reduced pressure to obtain 5-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride as a colorless solid (2.5 g, 78%).

Aufarbeitung

  1. additionmixed for 10 minutes
  2. distillationthe solvent was distilled off under reduced pressure
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionTo the residue was added isopropyl alcohol
  5. filtrationthe precipitate was collected by filtration
  6. washThe precipitate was washed sequentially with isopropyl alcohol and diethyl ether
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-3c01014afba649549ba72d67538716f5
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07820673B2

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