HRID480999

反应详情

EQUATION

反应方程式

HRID 480999 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 3-oxo-5-[2-[[2-(tritylamino)ethoxy]methyl]phenyl]pentanoate (3.33 g, 6.38 mmol), 2,6-dichlorobenzaldehyde (1.12 g, 6.38 mmol), acetic acid (0.5 ml), piperidine (0.5 ml) and benzene (50 ml) was stirred for 4 hours at reflux temperature azeotropically. The reaction mixture was quenched with water (40 ml) and the whole was extracted with Et2O (20 ml×2). The combined extracts were washed with brine, dried over MgSO4, and concentrated in vacuo to afford the titled compound as a yellow oil. (quant.)

WORKUP

后处理

  1. temperatureat reflux temperature azeotropically
  2. customThe reaction mixture was quenched with water (40 ml)
  3. extractionthe whole was extracted with Et2O (20 ml×2)
  4. washThe combined extracts were washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo