(5-Nitro-2-sulfanylphenyl)methanol → HCID 19045546, Verbindung

HRID 1781379Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1781379
[SH:1][C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=1[CH2:4][OH:5].N1C=CC=CC=1[CH2:19][CH2:20][CH:21]1[CH2:26][C:25](=O)[CH2:24][CH2:23][NH:22]1>C(Cl)(Cl)Cl>[N+:10]([C:7]1[CH:8]=[CH:9][C:2]2[S:1][C:25]3([CH2:24][CH2:23][N:22]([CH2:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=4)[CH2:21][CH2:26]3)[O:5][CH2:4][C:3]=2[CH:6]=1)([O-:12])=[O:11]

Komponenten

4

Edukt 2

HCID 54329580(5-Nitro-2-sulfanylphenyl)methanolHCID 86746766HCID 86746766, Verbindung

Produkt 1

HCID 19045546HCID 19045546, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

2-Mercapto-5-nitrobenzyl alcohol (150 mg, 0.81 mmol) and 208 mg (0.80 mm) of N-[2-(2'-pyridyl ethyl]-4-piperidone was dissolved in 5 mL of CHCl3. HCl Gas was bubbled in to saturate the solution, the mixture stirred at 25° C. for 2 days, then diluted with water and the pH adjusted to 10.0 with 40% aqueous NaOH. Extraction with CHCl3 and drying the organic phase (Na2SO4) gave after concentration and recrystallization from ethyl acetate 75 mg of an orange solid.

Aufarbeitung

  1. customHCl Gas was bubbled in
  2. concentrationto saturate the solution
  3. additiondiluted with water
  4. extractionExtraction with CHCl3
  5. dry with materialdrying the organic phase (Na2SO4)
  6. customgave
  7. concentrationafter concentration and recrystallization from ethyl acetate 75 mg of an orange solid

Quellen und Nachweise

ORD-Eintrag
ord-21f4820d09ec43eea37f1383b4e918e9
Quelldatensatz
uspto-grants-1997_05
Patentnummer
US05633247

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