HRID1061848

反应详情

EQUATION

反应方程式

HRID 1061848 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

n-Butyllithium (2.5 M, 16.9 mL) was added dropwise into a cold (−78° C.) solution of 2-bromo-6-methoxynaphthalene (10.0 g, 42.2 mmol), and THF (200 mL). The reaction mixture was stirred at −78° C. for 2 h, and then 2-fluoro-4-methoxybenzaldehyde (6.5 g, 42 2 mmol) in THF (10 mL) was added. The mixture was allowed to warm up to 0° C. stirred for 10 min, and then quenched with aqueous ammonium cholride. The mixture was poured into water, acidified with HCl (2N) and extracted with EtOAc. The organic extracts were dried over MgSO4. Evaporation and purification by flash chromatography (hexanes/EtOAc 3/1) gave a brown solid (12.2 g, 93% yield, m.p. 68-69° C.); MS m/e 312 (M+).

WORKUP

后处理

  1. temperatureto warm up to 0° C.
  2. stirringstirred for 10 min
  3. customquenched with aqueous ammonium cholride
  4. additionThe mixture was poured into water
  5. extractionextracted with EtOAc
  6. dry with materialThe organic extracts were dried over MgSO4
  7. customEvaporation and purification by flash chromatography (hexanes/EtOAc 3/1)