Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanethiol | HCID 878 | — |
| Reactant | HCID 19390523 | HCID 19390523 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178503578 | HCID 178503578 | 52.7% |
Reaction Steps
1370 g of 2-isopropyl-2-cyanohydrazinecarboxylic acid ethyl ester is placed into an autoclave, and 423 g of methyl mercaptan is injected. The temperature is held for 24 hours at 40° C. The resulting crystal mass is afterwards transferred to a 2.5 liter sulphonating flask, and heated in an oil bath for 2 1/2 hours at 120° C. There is then added to the reaction mixture cooled to 90° C 1.2 liters of water, whereupon the the reaction product precipitates in crystalline form. Crude 1-isopropyl-5-methylthio-3-hydroxy-1,2,4-thiazole is filtered off, and recrystallised from one liter of acetonitrile. There is obtained 730 g (52% of theory) of pure 1-isopropyl-5-methylthio-3-hydroxy-1,2,4-triazole, m.p. 88°-93° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04076938 |
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| Source dataset | uspto-grants-1978_02 |
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| ORD ID | ord-aa4e2b24f9d14cfab159c8c8480e4c73 |
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| Source note | uspto-grants-1978_02 |
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