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Hydrochloric Acid → HCID 14726996, Verbindung

HRID 329395
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 329395
Br.Cl[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[N:12]=[C:13]([NH2:17])[S:14][C:15]=2[CH3:16])=[CH:7][CH:6]=1.[C:18]1([N:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[CH:20][CH:19]=1.C(N(CC)CC)C.C(=O)([O-])[O-].[Na+].[Na+].[I-].[Na+].Cl>C(OCC)(=O)C.C(OCC)(=O)C.CO.CCOCC.C(O)C>[C:18]1([N:28]2[CH2:33][CH2:32][N:31]([CH2:3][CH2:4][C:5]3[CH:10]=[CH:9][C:8]([C:11]4[N:12]=[C:13]([NH2:17])[S:14][C:15]=4[CH3:16])=[CH:7][CH:6]=3)[CH2:30][CH2:29]2)[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[CH:20][CH:19]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 6

HCID 313Hydrochloric AcidHCID 13421-(1-Naphthyl)piperazineHCID 5238Sodium IodideHCID 8471TriethylamineHCID 10340Sodium CarbonateHCID 14726985HCID 14726985, Verbindung

Produkt 1

HCID 14726996
HCID 14726996, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 702EthanolLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 21584119Ethylacetate methanolLösungsmittel

Versuchsvorschrift

To a 35 ml round-bottomed flask equipped with condenser and N2 inlet were added 0.81 g (2.80 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-amino-5-methylthiazole hydrobromide, 0.59 g (2.80 mmol) of N-(1-naphthyl)piperazine, 0.78 ml (5.60 mmol) of triethylamine, 0.30 g (2.80 mmol) of sodium carbonate, 2 mg of sodium iodide, and 10 ml of ethanol. The reaction was heated at reflux for 5 days, cooled, and the reaction taken up in ethyl acetate, washed with water and brine, dried over sodium sulfate, and evaporated to an oil. The oil was chromatographed on silica gel using ethyl acetate/methylene chloride as eluent to give a white solid. The solid was taken up in ethyl acetate/methanol, ether saturated with HCl added, the precipitate filtered, washed with ether, and dried to give a white solid, 0.82 g (54%), m.p. 160°-165° C.

Aufarbeitung

  1. customTo a 35 ml round-bottomed flask equipped with condenser and N2 inlet
  2. temperatureThe reaction was heated
  3. temperatureat reflux for 5 days
  4. temperaturecooled
  5. washwashed with water and brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated to an oil
  8. customThe oil was chromatographed on silica gel
  9. customto give a white solid
  10. filtrationthe precipitate filtered
  11. washwashed with ether
  12. customdried
  13. customto give a white solid, 0.82 g (54%), m.p. 160°-165° C.

Quellen und Nachweise

ORD-Eintrag
ord-80c719e6475347e6837b77931b0dc6a5
Quelldatensatz
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04891375

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