反应详情

4-trifluoromethoxybenzoic acid hydrazide (1.1 g, 5.0 mmol) and S-methyl N-[4-hydroxy-phenyl]isothiourea hydroiodide (1.55 g, 5.0 mmol) were suspended in 10 mL of anhydrous pyridine. The reaction mixture was refluxed for 24 hours, during which time it changed color from yellow into orange-red. Then it was cooled down to ambient temperature and poured with stirring into 150 mL of ice-water. The aqueous layer was decanted and the resulting residue was purified by silica gel chromatography using 1:1 mixture of ethyl acetate/hexane. Solvent was removed in vacuo to give the title product as a pinkish-grey solid (684.0 mg). 40.6% yield.

1. temperatureThe reaction mixture was refluxed for 24 hours, during which time it
2. additionpoured
3. customThe aqueous layer was decanted
4. customthe resulting residue was purified by silica gel chromatography
5. addition1:1 mixture of ethyl acetate/hexane
6. customSolvent was removed in vacuo