HRID922213

反应详情

EQUATION

反应方程式

HRID 922213 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a 25 mL RB flask fitted with magnetic stirrer was charged with 10 mL of dichloromethane. To the stirred solvent was added ethyl 3-(2-fluoro-4-methoxyphenyl)propanoate (0.45 g, 2 mmol). The reaction mixture was cooled to 0° C. and boron tribromide (0.45 mL) was added drop wise. After stirred for 30 minutes, the reaction mixture was quenched with ethanol (1 mL) at 0° C. by slow addition. The reaction mixture was concentrated to distill off the solvent; ethyl acetate (10 mL) was added. The organic layer was washed with saturated NaHCO3 solution (10 mL), followed by brine solution (10 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The product was obtained as colorless oil (0.421 g, yield: 99.75%). 1H NMR (300 MHz, CDCl3): δ 6.93-6.99 (t, 1H), 6.43-6.48 (m, 2H), 5.54 (s, 1H), 4.02-4.09 (q, 2H), 2.79-2.85 (t, 2H), 2.50-2.55 (t, 2H), 1.14-1.19 (t, 3H).

WORKUP

后处理

  1. customTo a 25 mL RB flask fitted with magnetic stirrer
  2. customthe reaction mixture was quenched with ethanol (1 mL) at 0° C. by slow addition
  3. concentrationThe reaction mixture was concentrated
  4. distillationto distill off the solvent
  5. additionethyl acetate (10 mL) was added
  6. washThe organic layer was washed with saturated NaHCO3 solution (10 mL)
  7. dry with materialThe organic layer was dried over anhydrous Na2SO4
  8. customthe solvent was removed under reduced pressure