Water → HCID 178473548, compound

Participants

Reaction Steps

302 g. (2.78 moles) of ethyl chloroformate was added to 2 moles of S-ethylisothiourea hydrochloride in 800 ml. of water and 200 ml. of acetonitrile. A 25% solution of sodium hydroxide was added dropwise so rapidly that, with external cooling, a temperature of +25° C. was not exceeded. The solution of sodium hydroxide was added for as long as the pH value did not rise above 8. Stirring was effected for a further 80 minutes during which control of the pH value was continued. If necessary, a little more solution of sodium hydroxide was added. A two phase system, aqueous and organic, resulted. The product was isolated from the organic phase by extraction with methylene chloride and concentration in vacuo to a light yellow oil.

Provenance & Evidence