HRID368917

反应详情

EQUATION

反应方程式

HRID 368917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Table 1, Entry 11. In the reaction tube were mixed 4-acetylphenyl triflate (0.268 g, 1.0 mmol), phenyltributyltin (0.441 g, 1.2 mmol), Pd2 dba3 (0.00916 g, 0.010 mmol), triphenylarsine (0.0245 g, 0.080 mmol), lithium chloride (0.127 g, 3.0 mmol) and 1.0 ml NMP.under nitrogen. The contents of the flask were irradiated for 2.50 min with an effect of 50 W. After cooling, addition of 1 M aqueous KF (4 ml) with stirring for 120 min, were followed by dilution (DCM) and filtration through a pad of celite. The filtrate was washed with water (25 ml). Additional extraction of the aqueous phase was performed with DCM (2×25 ml). The combined extracts were washed with 25 ml saline and concentrated to an oil. The crude product was purified by column chromatography on silica gel using i-hexane/ethyl acetate (10/1) as the eluent. The yield was 68% (white solid).

WORKUP

后处理

  1. customThe contents of the flask were irradiated for 2.50 min with an effect of 50 W
  2. temperatureAfter cooling
  3. filtrationwere followed by dilution (DCM) and filtration through a pad of celite
  4. washThe filtrate was washed with water (25 ml)
  5. extractionAdditional extraction of the aqueous phase
  6. washThe combined extracts were washed with 25 ml saline
  7. concentrationconcentrated to an oil
  8. customThe crude product was purified by column chromatography on silica gel