反应详情

Diethyl [(2,3,4-trifluoroanilino)(mercapto)methylene]malonate sodium salt (68.5 g) was dissolved in N,N-dimethylformamide (200 ml) and thereto p-methoxybenzyl chloride (28.9 g) was added dropwise at 3° to 5° C. over a period of 5 minutes. After the reaction mixture was stirred at room temperature for 1 hour and evaporated to dryness under reduced pressure, water was added to the residue and the mixture was extracted with chloroform. After the extract was washed with a NaCl solution and dried over magnesium sulfate, the solvent was distilled off under reduced pressure to give the title compound (82.9 g) as colorless solid, which was then recrystallized from a mixed solvent of haxane - benzene.

1. customevaporated to dryness under reduced pressure, water
2. additionwas added to the residue
3. extractionthe mixture was extracted with chloroform
4. washAfter the extract was washed with a NaCl solution
5. dry with materialdried over magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure