HRID2277602

反应详情

EQUATION

反应方程式

HRID 2277602 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium bis(trimethylsilyl) amide (2 mL, 2 M in THF, 2 mmol) was added dropwise at 0° C. to a solution of 5-chloro-2,3-dihydro-isoindol-1-one (0.34 g, 2 mmol) in THF (10 mL). After stirring for 10 min, 1-bromomethyl-4-methoxy-benzene (0.52 g, 2.6 mmol) was added dropwise. The resulting reaction mixture was allowed to stir at room temperature for 48 hours before quenching with saturated aqueous ammonium chloride solution. After extraction with EtOAc, the organic layer was washed with brine, dried over anhy. Na2SO4, filtered and concentrated in vacuo to give the crude product (0.6 g, 100%) as a yellow oil. MS: 288.0 (M+H+). It was used directly in the next step, without further purification.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. stirringto stir at room temperature for 48 hours
  3. custombefore quenching with saturated aqueous ammonium chloride solution
  4. extractionAfter extraction with EtOAc
  5. washthe organic layer was washed with brine
  6. customdried over anhy
  7. filtrationNa2SO4, filtered
  8. concentrationconcentrated in vacuo