반응 #63151
ord-4664c9396b2a4a6ea9726df8d45d1fc4
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타prepared by the procedure of South African Patent Application No
- 2기타to 37° C
- 3온도, the suspension was refluxed for 6 hours
- 4온도cooled to 25° C.
- 5기타to yield a precipitate
- 6여과The mixture was filtered
- 7세척washed with water
- 8기타the isolated solid was recrystallized from acetonitrile
실험 절차
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 No. 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.