Triethylamine → HCID 178521527, Verbindung

HRID 606449Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 606449
[NH:1]1[CH:5]=[N:4][C:3]([SH:6])=[N:2]1.I[CH2:8][CH2:9][OH:10].C(N(CC)CC)C>C(O)C>[NH:1]1[CH:5]=[N:4][C:3]([S:6][CH2:8][CH2:9][OH:10])=[N:2]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 12225IodoethanolHCID 178527894HCID 178527894, Verbindung

Produkt 1

HCID 178521527HCID 178521527, VerbindungAusbeute 35 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 1H-1,2,4-triazole-3-thiol (14.7 g, 145 mmol), 2-iodoethanol (25.0 g, 145 mmol) and triethylamine (14.7 g, 145 mmol) in ethanol (400 mL) was stirred at 80° C. for 15 hr. The reaction mixture was concentrated under reduced pressure, and the residue was acidified with water and 1N hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated. The obtained oil was purified by silica gel column chromatography (10%-100% ethyl acetate/hexane) to give the title compound as a colorless oil (7.30 g, 35%).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe obtained oil was purified by silica gel column chromatography (10%-100% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-062d5293625f490eb1a0a19b3947a226
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07915267B2

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