Ammonia → 1-Trimethylsilyl-1,2,4-triazole

HRID 435200

Reaktionsgleichung

Reaktionsgleichung von HRID 435200
[CH3:1][Si:2]([CH3:9])([CH3:8])[NH:3][Si](C)(C)C.N1[CH:14]=[N:13][CH:12]=[N:11]1.N>S1(C2C(=CC=CC=2)C(=O)N1)(=O)=O>[CH3:1][Si:2]([CH3:9])([CH3:8])[N:3]1[CH:14]=[N:13][CH:12]=[N:11]1

Komponenten

5

Edukt 3

HCID 222Ammonia2×HCID 92571H-1,2,4-TriazoleHCID 13838Hexamethyldisilazane

Produkt 1

HCID 875581-Trimethylsilyl-1,2,4-triazoleAusbeute 124,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5143SaccharinKatalysator

Reaktionsbedingungen

Temperatur
126 °C

Versuchsvorschrift

23.4 ml (0.11 mole) of hexamethyldisilazane were added to a mixture consisting of 10.35 g (0.15 mole) of 1,2,4-triazole and 127 mg (0.75 mmole) of saccharin heated to 126° C. and evolution of ammonia started immediately. After refluxing for 30 minutes, the calculated amount of ammonia was evolved as determined by the method described in Example 1A. Vacuum distillation yielded 19.37 g (91.6%) of 1-trimethylsilyl-1,2,4-triazole boiling at 76.5°-78.0° C. at 12 mm Hg and nD 25=1.4592.

Aufarbeitung

  1. temperatureAfter refluxing for 30 minutes
  2. distillationVacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-444c485f5de048b295ef616b6fd3e31c
Quelldatensatz
uspto-grants-1983_08
Patentnummer
US04400509

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