反应详情

温度

65 °C

To a 25 mL RB flask fitted with magnetic stirrer was charged 10 mL of methanol. To the stirred solvent was added 2-cyano-3-(4-hydroxy-phenyl)-propanoic acid (0.5 g, 2.62 mmol), followed by methanesulfonic aid (0.5 mL, 7.69 mmol). After addition, the RM was refluxed at 65° C. for 1 h. After 1 h, the solvent was evaporated, water (20 mL) was added and the organic layer was extracted with ethyl acetate (15 mL×2). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The product was obtained as brown liquid. (0.3 g, yield: 55.8%): MS (ESI, 120 eV): m/z=204.1 (M−H)+.

1. customTo a 25 mL RB flask fitted with magnetic stirrer
2. additionAfter addition
3. customthe solvent was evaporated
4. additionwater (20 mL) was added
5. extractionthe organic layer was extracted with ethyl acetate (15 mL×2)
6. dry with materialThe organic layer was dried over anhydrous Na2SO4
7. customthe solvent was removed under reduced pressure
8. customThe product was obtained as brown liquid