1,2-dihydro-1-(o-methoxyphenyl)-5H-tetrazole-5-thione synthesis
- Product Name:1,2-dihydro-1-(o-methoxyphenyl)-5H-tetrazole-5-thione
- CAS Number:15182-67-9
- Molecular formula:C8H8N4OS
- Molecular Weight:208.24
3288-04-8
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Yield:15182-67-9 33.82%
Reaction Conditions:
Stage #1: 1-isothiocyanato-2-methoxybenzenewith sodium azide in water; for 2 h;Reflux;
Stage #2: with hydrogenchloride in water; pH=2;
Steps:
Synthesis of thione L.
o-Methoxyphenyl isothiocyanate(6.431 g, 39 mmol) was added to a solution ofNaN3 (2.53 g, 39 mmol) in 2 (50 mL) at 20°. Thereaction mixture was refluxed for 2 h, cooled to 20°,and filtered to remove nondissolved impurities. A 10%aqueous solution of HCl was added with stirring to theobtained solution to pH 2. The precipitate formed wasfiltered off, washed with water (200 mL), and dried at353 K. The product for X-ray diffraction analysis wasrecrystallized from ethanol. The yield of L as whitecrystals with mp = 162-164° (with decomposition)was 7.036 g (33.82%).
References:
Askerov;Magerramov;Osmanov;Baranov;Borisova;Samsonova;Borisov [Russian Journal of Coordination Chemistry,2019,vol. 45,# 2,p. 112 - 118][Koord. Khim.,2019,vol. 45,# 2,p. 99 - 105,7]
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