反应详情

In 6.2 ml of methylene chloride were dissolved 310 mg (1.37 mmol.) of 2,3,4-trimethoxyphenylacetic acid and 289 mg (1.64 mmol.) of methyl 1-piperazinecarbodithioate. To the solution was added 395 mg (1.92 mmol.) of dicyclohexylcarbodiimide. The mixture was stirred at room temperature for 1 hour. A precipitated solid was removed by filtration, and to the filtrate were added methylene chloride and 1-N hydrochloric acid. The organic solvent portion was taken out, washed with a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and placed under reduced pressure to distill off the solvent. The residue was purified over a silica gel column. The obtained oil was crystallized from a mixture of ethanol and hexane, yielding 257 mg of the desired compound as a white crystalline product, m.p. 119°-120° C., yield 48.8%.

1. customA precipitated solid was removed by filtration
2. additionto the filtrate were added methylene chloride and 1-N hydrochloric acid
3. washwashed with a saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. distillationto distill off the solvent
6. customThe residue was purified over a silica gel column
7. customThe obtained oil was crystallized from a mixture of ethanol and hexane