HRID2096635

反应详情

EQUATION

反应方程式

HRID 2096635 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 2-Acetyl-4-bromophenol (1.754 g, 8.16 mmol), 2-(tetrahydrofuran-2-yl)acetaldehyde (2.1 g) and purrolidine (0.4 mL) in MeOH was heated to reflux for 2 h. The reaction mixture was cool down to room temperature and evaporated. The residue was dissolved in EA, washed with 1 M HCl, 1 M NaOH (2×50 mL), brine (100 mL) successively, then, dried over anhydrous Na2SO4, and filtered, and concentrated. The residue was purified by flash chromatography on silica gel eluting with EA in hexane (0-20%) to give 6-bromo-2-((tetrahydrofuran-2-yl) methyl)chroman-4-one (464 mg); MS ESI +ve m/z 311 (M+H)+.

WORKUP

后处理

  1. temperatureto reflux for 2 h
  2. customevaporated
  3. dissolutionThe residue was dissolved in EA
  4. washwashed with 1 M HCl, 1 M NaOH (2×50 mL), brine (100 mL) successively
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by flash chromatography on silica gel eluting with EA in hexane (0-20%)