Hydrogen chloride-ethyl acetate → N-[1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Trihydrochloride

HRID 1978459Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1978459
[S:1]1[CH:5]=[C:4]([CH2:6][N:7]2[CH2:12][CH2:11][CH:10]([CH2:13][NH:14][C:15]([C:17]3[S:27][C:26]4[N:28]5[C:19](=[CH:20][N:21]=[C:22]5[CH:23]=[CH:24][CH:25]=4)[CH:18]=3)=[O:16])[CH2:9][CH2:8]2)[N:3]=[CH:2]1.[ClH:29].C(OCC)(=O)C>C(O)C>[ClH:29].[ClH:29].[ClH:29].[S:1]1[CH:5]=[C:4]([CH2:6][N:7]2[CH2:8][CH2:9][CH:10]([CH2:13][NH:14][C:15]([C:17]3[S:27][C:26]4[N:28]5[C:19](=[CH:20][N:21]=[C:22]5[CH:23]=[CH:24][CH:25]=4)[CH:18]=3)=[O:16])[CH2:11][CH2:12]2)[N:3]=[CH:2]1

Komponenten

4

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 21993714N-(1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide

Produkt 1

HCID 21994197N-[1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide TrihydrochlorideAusbeute 28 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of N-[1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol was added 2 ml (8.0 mM) of 4N-HCl/ethyl acetate. The solvent was distilled off under reduced pressure and the residue was diluted with ether. The crystals that formed were harvested by filtration and rinsed with ethanol and diethyl ether to provide the title compound as orange-colored crystals (150 mg, 28%).

Aufarbeitung

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionthe residue was diluted with ether
  3. customThe crystals that formed
  4. filtrationwere harvested by filtration
  5. washrinsed with ethanol and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-2ddab0d055624d3a97c86614a726e537
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06235731B1

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