HRID63637

反应详情

EQUATION

反应方程式

HRID 63637 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (2-carboxyethyl)triphenylphosphonium bromide (14.8 g, 35.7 mmol) in THF (40 mL) was added NaHMDS (35.8 mL, 71.5 mmol) at −20° C., and the reaction was stirred for 20 min. 4-Fluoro-3-methoxybenzaldehyde (5.0 g, 32.5 mmol) was added to the reaction at −78° C., and the reaction was stirred overnight while warming to rt. The reaction was diluted with water (30 mL) and extracted with EtOAc (3×30 mL). Organics were washed with brine (30 mL), dried (Na2SO4), and concentrated to give 6.0 g (88%) of the crude title compound as a yellow solid. [M+H] Calc'd for C11H11FO3, 211. Found, 211.

WORKUP

后处理

  1. stirringthe reaction was stirred overnight
  2. extractionextracted with EtOAc (3×30 mL)
  3. washOrganics were washed with brine (30 mL)
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated