Water → HCID 178514681, compound

Participants

Reaction Steps

To 2.9 g of potassium hydroxide dissolved in 45 ml of ethanol and 9 ml of water was added with stirring 4.0 g of carbon disulfide. This solution was then added dropwise to 300 ml of ethanol containing 11.8 g of 2-amino-4-chloro-5-sulfamylaniline. The reaction was refluxed for 5 hours and then concentrated in vacuo to a dark oil. Treatment with 50° C. water provided a solid which was removed by filtration. The filtrate was cooled with ice and acidified to pH 5.0 with acetic acid to yield a gray solid. Trituration of the solid with boiling methanol provided a solid which upon drying gave 5.6 g of pink crystals, m.p. 341°-343°.

Provenance & Evidence