HRID1662503

反应详情

EQUATION

反应方程式

HRID 1662503 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

A 500 mL round bottom flask was charged with 5-(2-fluoro-3-methoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione 77.B (5.00 g, 17.8 mmol) and THF (100 mL). The resulting slurry was cooled to 0° C., and to it was added ethylmagnesium bromide (available from Aldrich) (3.0 M/ether) (11.9 mL, 35.7 mmol) dropwise over 15 minutes. The cooling bath was removed, and the mixture was stirred for 1 hour at ambient temperature. The reaction was quenched with 1 N HCl and extracted with EtOAc. The combined organic layers were washed with brine, dried (MgSO4), and concentrated to afford 5-(1-(2-fluoro-3-methoxyphenyl)propyl)-2,2-dimethyl-1,3-dioxane-4,6-dione 77.C (5.17 g, 93.4% yield) as a yellow oil (5.2 g, 93%). The product thus obtained was used without further purification.

WORKUP

后处理

  1. customThe cooling bath was removed
  2. customThe reaction was quenched with 1 N HCl
  3. extractionextracted with EtOAc
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated