Chlorophenyl isocyanate → HCID 178518972, Verbindung

HRID 2226252Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2226252
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]=[C:9]=[O:10].C[Si]([N:15]=[N+:16]=[N-:17])(C)C>>[CH:5]1[CH:4]=[C:3]([N:8]2[NH:17][N:16]=[N:15][C:9]2=[O:10])[C:2]([Cl:1])=[CH:7][CH:6]=1

Komponenten

3

Edukt 2

HCID 76833Chlorophenyl isocyanateHCID 78378Azidotrimethylsilane

Produkt 1

HCID 178518972HCID 178518972, VerbindungAusbeute 78,1 %

Versuchsvorschrift

2-Chlorophenylisocyanate (7 g) and trimethylsilyl azide (7.9 g) were mixed and heated under refluxing for eight hours. The excessive trimethylsilyl azide was distilled off under reduced pressure and to the residue there were added 40 ml of methanol. Thereafter, the methanol was evaporated and the residue was purified by flush column chlomatography (hexane:ethyl acetate=2:1) to obtain the desired 1-(2-chlorophenyl)-5(4H)-tetrazolinone (7 g) having a melting point in the range of from 124.5° to 125.5° C.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder refluxing for eight hours
  3. distillationThe excessive trimethylsilyl azide was distilled off under reduced pressure and to the residue there
  4. additionwere added 40 ml of methanol
  5. customThereafter, the methanol was evaporated
  6. customthe residue was purified
  7. customby flush column chlomatography (hexane:ethyl acetate=2:1)

Quellen und Nachweise

ORD-Eintrag
ord-d4a2078f80cf4849ad577090be9300e4
Quelldatensatz
uspto-grants-1994_09
Patentnummer
US05347010

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