HRID1394226

反应详情

EQUATION

反应方程式

HRID 1394226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of sodium phenoxide (prepared from phenol and NaH) (6 mmol) in THF (3 mL) was added to a solution of the product from Step 1 (600 mg, 3.0 mmol) in THF (2 mL) and the resulting solution was heated to reflux overnight. The solution was cooled, poured into H2O and extracted with EtOAc. The organic layers were washed with H2O and brine, dried, filtered and concentrated to give a residue which was purified by column chromatography (5-80% EtOAc in hex) to give the title compound which was used directly in the next step. MS (ES+) m/e 260. [M+H]+.

WORKUP

后处理

  1. temperaturethe resulting solution was heated
  2. temperatureto reflux overnight
  3. temperatureThe solution was cooled
  4. extractionextracted with EtOAc
  5. washThe organic layers were washed with H2O and brine
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give a residue which
  10. customwas purified by column chromatography (5-80% EtOAc in hex)