HRID2251535

反应详情

EQUATION

反应方程式

HRID 2251535 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 2-methyl-2-[4-(2-{[4-(trifluoromethoxy)benzyl]amino}ethyl)phenoxy]propanoate (3.0 g; 7.05 mmol) in 8 ml of DMF was treated with 6-chloronicotinaldehyde (0.91 g; 6.42 mmol) and K2CO3 (0.97 g; 7.05 mmol). The reaction mixture was heated at 150C for 4 hr. Upon cooling, the mixture was partitioned between ethyl acetate and 0.05N HCl. The organic phase was washed with 0.05N HCl and brine, dried over sodium sulfate, filtered and concentrated. Purification by flash chromatography using ethyl acetate-hexane mixtures (5–50%) afforded the title compound (2.3 g; 68% yield).

WORKUP

后处理

  1. temperatureUpon cooling
  2. customthe mixture was partitioned between ethyl acetate and 0.05N HCl
  3. washThe organic phase was washed with 0.05N HCl and brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customPurification by flash chromatography