HRID1627958

反应详情

EQUATION

反应方程式

HRID 1627958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(3-methoxy phenyl)acetamide (41 mg, 0.25 mmol), n-butyl acrylate (64 mg, 0.50 mmol), 1,4-benzoquinone (27 mg, 0.25 mmol), AgNO3 (85 mg, 0.5 mmol), and [Pd(MeCN)4](BF4)2 (11 mg, 0.025 mmol) were sequentially added under air to a reaction tube equipped with a stir bar and a septum. A degassed aqueous solution containing TPGS-M-PEG-750 (1.0 mL, 2 wt %) was added by syringe and the resulting mixture vigorously stirred for 20 h. After this time, the contents of the flask were quenched with aqueous NaHCO3 and extracted with EtOAc. The solution obtained was filtered through the plug of silica gel and anhydrous MgSO4, and then concentrated by rotary evaporation. The residue was purified by flash chromatography, eluting with 50% EtOAc/hexanes to afford the product as an off-white solid (60 mg, 83%).

WORKUP

后处理

  1. customequipped with a stir bar
  2. additionwas added by syringe
  3. customAfter this time, the contents of the flask were quenched with aqueous NaHCO3
  4. extractionextracted with EtOAc
  5. customThe solution obtained
  6. filtrationwas filtered through the plug of silica gel and anhydrous MgSO4
  7. concentrationconcentrated by rotary evaporation
  8. customThe residue was purified by flash chromatography
  9. washeluting with 50% EtOAc/hexanes