HRID478774

反应详情

EQUATION

反应方程式

HRID 478774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of {3-(ethoxycarbonyl)-2-oxopropyl}triphenyl phosphonium chloride (21.34 g, 500 mmol) in water (450 mL) was added to a solution of sodium carbonate (3.1 g, 25.0 mmol) in 10 min (Note: A white precipitate was obtained immediately after the addition). This reaction mixture was stirred at room temperature overnight. The precipitate that obtained was filtered off through a sintered funnel. The precipitate was dissolved in dichloromethane (100 mL), dried over sodium sulfate and concentrated to yield a white solid 18.13 g (93%). This material was dried over phosphorus pentoxide overnight. 1H NMR (CDCl3) δ1.26 (t, 3H), 3.34 (s, 2H), 3.76-3.84 (d, 1H) 4.19 (m, 2H) and 7.48-7.68 (m, 15H, PhH).

WORKUP

后处理

  1. customA white precipitate was obtained immediately
  2. additionafter the addition)
  3. customThe precipitate that obtained
  4. filtrationwas filtered off through a sintered funnel
  5. dissolutionThe precipitate was dissolved in dichloromethane (100 mL)
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated