HRID660420

反应详情

EQUATION

反应方程式

HRID 660420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

While replacing with nitrogen, NaH (0.13 g, 0.0054 mol) was suspended in absolute THF (20 mL), and N,N-diethylphosphonoacetamide (1.36 g, 0.0054 mol)/absolute THF (10 mL) was added dropwise at 0° C. Then, 2-acetyl-7-(1-phenylethoxy)benzo[b]furan (1.0 g, 0.0036 mol)/absolute THF (20 mL) was added dropwise. After stirring for 6 h while allowing to warm to room temperature, the disappearance of the starting materials was confirmed by TLC. The reaction mixture was poured into saturated aqueous NH4Cl solution, mixed and THF was evaporated under reduced pressure. The residue was extracted with ethyl acetate, washed with brine, dried over absolute magnesium sulfate, and evaporated under reduced pressure to give a pale-yellow oil. The obtained oil was purified by column chromatography to give the title compound as a pale-yellow oil. (0.75 g, 55.6%)

WORKUP

后处理

  1. additionmixed
  2. customTHF was evaporated under reduced pressure
  3. extractionThe residue was extracted with ethyl acetate
  4. washwashed with brine
  5. dry with materialdried over absolute magnesium sulfate
  6. customevaporated under reduced pressure
  7. customto give a pale-yellow oil
  8. customThe obtained oil was purified by column chromatography