反应详情

A mixture of 1063.4 g of (1-methylethyl)-2-(aminosulfonyl)-4-chlorobenzoate, 590.4 g of butylisocyanate, 590.4 g of potassium carbonate and 10.8 L of 2-butanone was heated at reflux overnight. After cooling to ambient temperature, the reaction mixture was divided into two portions. Each portion was poured into 10 L of ice-water. The aqueous mixtures were extracted with 9 L each of methylene chloride. The combined aqueous phases were acidified to pH 1.0 with concentrated hydrochloric acid. The resulting solids were collected and dried to give 714.6 g of the title compound, m.p. 129°.132° C.

1. temperaturewas heated
2. temperatureat reflux overnight
3. extractionThe aqueous mixtures were extracted with 9 L each of methylene chloride
4. customThe resulting solids were collected
5. customdried