反应详情

To a solution containing 12.2 g of trichloromethyl chloroformate in 130 ml of p-dioxane was added portionwise 16 g of 2-[(phenylmethyl)thio]benzoic acid, hydrazide [prepared by the procedure of South African Patent Application 838,416 (1983)] to cause a slight exotherm to 37° C. After stirring at ambient temperature for 0.5 hr., the suspension was refluxed for 6 hours, then cooled to 25° C. and poured onto excess ice/water to yield a precipitate. The mixture was filtered, washed with water and the isolated solid was recrystallized from acetonitrile to yield 14 g of the subject compound; m.p. 169°-172° C.

1. customprepared by the procedure of South African Patent Application 838,416 (1983)]
2. customto 37° C
3. temperature, the suspension was refluxed for 6 hours
4. temperaturecooled to 25° C.
5. customto yield a precipitate
6. filtrationThe mixture was filtered
7. washwashed with water
8. customthe isolated solid was recrystallized from acetonitrile