HRID1362257
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 37 °C
PROCEDURE
实验过程
To a solution of 2-hydroxy-3-trifluoromethoxybenzaldehyde (1.00 g, 4.82 mmol) in DMF (10 mL), was added K2CO3 (1.46 g, 10.6 mmol) followed by iodoethane (0.57 mL, 7.24 mmol) and the mixture was heated to 37° C. for 6 h. The reaction was quenched by the addition of H2O (40 mL) and the mixture was extracted with EtOAc (3×100 mL). The combined organics were washed with brine (2×100 mL), dried (Na2SO4) and concentrated to yield the title compound (1.17 g, quant.) as an orange oil: 1H NMR (300 MHz, DMSO-d6) δ 10.31 (s, 1H), 7.77 (m, 2H), 7.38 (t, J=8.1 Hz, 1H), 4.19 (q, J=6.9 Hz, 2H), 1.36 (t, J=6.9 Hz, 3H).
WORKUP
后处理
- customThe reaction was quenched by the addition of H2O (40 mL)
- extractionthe mixture was extracted with EtOAc (3×100 mL)
- washThe combined organics were washed with brine (2×100 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated