反应详情

温度

55 °C

To a solution of methyl 4-cyano-3-methylbenzoate (36 mg, 0.205 mmol) in 1,4-dioxane (0.5 mL) and water (0.500 mL), was added sodium hydrogen sulfide (0.019 mL, 0.616 mmol) and triethylamine hydrochloride (170 mg, 1.233 mmol). The reaction mixture was heated at 55° C. overnight. The reaction was allowed to cool and water was added. The mixture was extracted with EtOAc. The combined organic layers were dried (Na2SO4), filtered and the solvent was evaporated in vacuo to give the product as a yellow solid. LCMS calc.=210.1; found=210.2 (M+1)+. 1H NMR (500 MHz, CDCl3) 7.86 (s, 1H); 7.84 (d, J=8.1 Hz, 1H); 7.42 (d, J=7.9 Hz, 1H); 7.16 (s, 2H); 3.93 (s, 3H); 2.51 (s, 3H).

1. temperatureto cool
2. extractionThe mixture was extracted with EtOAc
3. dry with materialThe combined organic layers were dried (Na2SO4)
4. filtrationfiltered
5. customthe solvent was evaporated in vacuo