Reaktion #630249

Reaktionsgleichung

4-methyl-α-tetralone

Hydroxylamine hydrochloride

Tellurium dioxide

ethanol

→

dark red needles

Ausbeute 66.3%

3-Chloro-5-methylnaphth[2,1-c]-1,2,5-oxatellurazole

Ausbeute 66.3%

Lösungsmittel

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe stirred mixture heated briefly
2. 2
   SonstigeThe solid mass of crystalline product was collected
3. 3
   Waschenwashed well with water
4. 4
   Sonstigedried in a vacuum oven at 90° C.

Vorschrift

Tellurium dioxide (79.5 g=0.5 mole) was dissolved in concentrated hydrochloric acid (200 ml). Hydroxylamine hydrochloride (35 g=0.5 mole) was added and then ethanol to bring the total volume to 2000 ml. To the slightly turbid solution was added 4-methyl-α-tetralone (80 g=0.5 mole) and the stirred mixture heated briefly to boil. The clear deep red solution was then kept overnight at room temperature. The solid mass of crystalline product was collected, washed well with water and dried in a vacuum oven at 90° C. to give a first crop (111.1 g) of dark red needles. The filtrate was heated once again and kept at room temperature for 24 hours. A second crop of 14.3 g crude product was obtained. The well-dried product was placed into a Soxhlet thimble and extracted with methylene chloride. The majority of purified product crystallized from the solvent during the course of the extraction to give a yield of 97.0 g=58.3% of theory, m.p. 196°-198° C. Elemental analyses results were in agreement with the structural formula. The ultraviolet and visible spectra in dichloromethane showed three maxima.

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