Ethanethiol → HCID 178477363, compound

19.8 g (0.2 mole) of 1-isopropyl-1-cyanohydrazine is added dropwise to a solution of 16.0 g (0.4 mole) of sodium hydroxide and 12.4 g (0.2 mole) of ethyl mercaptan in 75 ml of water. Into the resulting white emulsion there is then introduced 19.8 g (0.2 mole) of phosgene at room temperature, and an exothermic reaction occurs. The reaction mixture cooled to room temperature, from which has separated out a white-yellow precipitate, is extracted with methylene chloride and the extract is dried with sodium sulphate. After removal of the methylene chloride by evaporation in vacuo, the crude product is purified by dissolving it in 50 ml of methanol, treating the solution with animal charcoal and crystallising the resulting product at -50° C. There is obtained 1-isopropyl-3-hydroxy-5-ethylthio-1,2,4-triazole, m.p. 109°-114° C.

1. customan exothermic reaction
2. customhas separated out a white-yellow precipitate
3. extractionis extracted with methylene chloride
4. dry with materialthe extract is dried with sodium sulphate
5. customAfter removal of the methylene chloride
6. customby evaporation in vacuo
7. customthe crude product is purified
8. dissolutionby dissolving it in 50 ml of methanol
9. additiontreating the solution with animal charcoal
10. customcrystallising the resulting product at -50° C

ORD record

ord-4925f2f796524207bfbb5bc1c62a6864

Source dataset

uspto-grants-1977_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04055572