Tributyltin azide → HCID 178493528, Verbindung

HRID 1938681

Reaktionsgleichung

Reaktionsgleichung von HRID 1938681
[C:1]([CH:3]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:4][C:5]([NH:7][C:8]1[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=1[O:18][CH3:19])=[O:6])#[N:2].C([Sn]([N:39]=[N+:40]=[N-:41])(CCCC)CCCC)CCC>O1CCOCC1>[NH:39]1[C:1]([CH:3]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH2:4][C:5]([NH:7][C:8]2[C:9]([O:18][CH3:19])=[CH:10][C:11]([O:16][CH3:17])=[CH:12][C:13]=2[O:14][CH3:15])=[O:6])=[N:2][N:41]=[N:40]1

Komponenten

4

Edukt 2

HCID 4984872Tributyltin azideHCID 86748282beta-cyano-N-(2,4,6-trimethoxyphenyl)benzene propanamide

Produkt 1

HCID 178493528HCID 178493528, VerbindungAusbeute 34,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a suspension of the material from step (a) (5.1 g, 0.016 mol) in dioxane (150 mL) at room temperature was added tri-n-butyltin azide (9.36 g, 0.016 mol) under N2 with stirring. The resulting solution was heated to reflux for 24 hours. The solution was then cooled and concentrated in vacuo. The residue was redissolved in ether and HCl gas was then passed through the'solution for 30 minutes. This was then concentrated in vacuo to give β-(1H-tetrazol-5-yl)-N-(2,4,6-trimethoxyphenyl)benzene propanamide as a white solid (2.1 g) which was used without further purification.

Aufarbeitung

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 24 hours
  3. temperatureThe solution was then cooled
  4. concentrationconcentrated in vacuo
  5. dissolutionThe residue was redissolved in ether
  6. concentrationThis was then concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-50ccdb9620604ecebd0a2e45768a7235
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05693657

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