Ethanethiol → HCID 178477363, compound

19.8 g (0.2 mole) of 1-isopropyl-1-cyanohydrazine is added dropwise to a solution of 8.0 g (0.2 mole) of sodium hydroxide and 12.4 g (0.2 mole) of ethyl mercaptan in 150 ml of water, whereby a slightly exothermic reaction occurs. An addition is then made dropwise, at 20° to 25° C, of 21.7 g (0.2 mole) of chloroformic acid ethyl ester, and the reaction mixture is subsequently refluxed for 11/2 hours. On cooling of the reaction mixture to room temperature, there is precipitated an oil. The reaction mixture is extracted twice with 150 ml of chloroform each time; the extract is dried over sodium sulphate and the solvent is evaporated off in vacuo. The white crystalline residue is dissolved in 75 ml of methanol, the solution is treated with animal charcoal and crystallisation is effected at -70° C. There is obtained in this manner 1-isopropyl-3-hydroxy-5-ethylthio-1,2,4-triazole, m.p. 109°-113° C.

1. customa slightly exothermic reaction
2. additionAn addition
3. temperaturethe reaction mixture is subsequently refluxed for 11/2 hours
4. customthere is precipitated an oil
5. extractionThe reaction mixture is extracted twice with 150 ml of chloroform each time
6. dry with materialthe extract is dried over sodium sulphate
7. customthe solvent is evaporated off in vacuo
8. dissolutionThe white crystalline residue is dissolved in 75 ml of methanol
9. additionthe solution is treated with animal charcoal and crystallisation
10. customis effected at -70° C

ORD record

ord-2abcb051a56e4fd4947ff0d4c851db2b

Source dataset

uspto-grants-1977_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04055572