Water → HCID 178458783, Verbindung

HRID 2236540Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2236540
[N:1]([CH2:4][C:5]1[CH:10]=[C:9]([OH:11])[C:8]([O:12][CH2:13][CH2:14][CH3:15])=[CH:7][N:6]=1)=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O>O1CCCC1>[NH2:1][CH2:4][C:5]1[CH:10]=[C:9]([OH:11])[C:8]([O:12][CH2:13][CH2:14][CH3:15])=[CH:7][N:6]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 1784587892-Azidomethyl-5-propoxy-pyridin-4-ol

Produkt 1

HCID 178458783HCID 178458783, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 2-azidomethyl-5-propoxy-pyridin-4-ol (9.70 g, 46.6 mole), is then suspended in 120 mL of tetrahydrofuran and treated with triphenylphosphine (12.22 g, 46.6 mmole) after stirring for 10 mins at ambient temperature water is added (12.6 mL, 15 equivalents) and the reaction mixture is stirred at ambient temperature overnight. The solids gradually dissolved followed by the formation of a precipitate. The resulting solid is filtered, washed with fresh 10:1 tetrahydrofuran:water and dried to give, 5.92 g, (69%), mp 159-60° C.; MS (ES+): m/z 183.3 (M+H).

Aufarbeitung

  1. additionis added (12.6 mL, 15 equivalents)
  2. dissolutionThe solids gradually dissolved
  3. filtrationThe resulting solid is filtered
  4. washwashed with fresh 10:1 tetrahydrofuran
  5. dry with materialwater and dried
  6. customto give

Quellen und Nachweise

ORD-Eintrag
ord-04458ab4061e476fa4970e21fc5eca61
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07713994B2

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