Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Azide | HCID 33557 | — |
| Edukt | Ethyl 4-isothiocyanatobenzoate | HCID 71003 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 178524450 | HCID 178524450 | 120,3% |
Reaktionsschritte
Then, 31 g of ethyl p-isothiocyanatobenzoate and 11.7 g of sodium azide were dispersed in 300 ml of water and the dispersion was refluxed for 5 hours. The reaction mixture was cooled to room temperature and acidified (pH about 2) by the addition of concentrated hydrochloric acid. Crystals of 1-(4-ethoxycarbonylphenyl)-5-mercaptotetrazole thus deposited were collected by filtration and after adding thereto 25 g of sodium hydroxide and 500 ml of water, the mixture was stirred for 30 minutes at 70° C. The reaction mixture was cooled to room temperature, neutralized by the addition of concentrated hydrochloric acid, and crystals thus deposited were collected by filtration and recrystallized from methanol to provide 40 g of 1-(4-carboxyphenyl)-5-mercaptotetrazole. The yield was 48% and the melting point was 198° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04737452 |
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| Quelldatensatz | uspto-grants-1988_04 |
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| ORD ID | ord-09ca77bdf0cc43acaceb3c71a6aa069e |
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| Quellennotiz | uspto-grants-1988_04 |
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