HRID1179477

反应详情

EQUATION

反应方程式

HRID 1179477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (2E)-3-(4-{[(benzyloxy)carbonyl]amino}-2-fluorophenyl)prop-2-enyl diazoacetate (2.26 g, 6.12 mmol) in toluene (125 mL) was added dropwise over 14 h to a refluxing solution of bis-(N-t-butylsalicylaldiminato)copper(II) (0.254 g, 0.61 mmol, prepared as described by R. G. Charles, J. Org. Chem. 1957, 22, 677) in 125 mL of toluene. After the addition was complete, the reaction mixture was heated another hour at reflux, then cooled, filtered and concentrated. The crude oil was purified by column chromatography (0-0.5% MeOH-DCM) to provide the title compound as a yellow solid.

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturethe reaction mixture was heated another hour
  3. temperatureat reflux
  4. temperaturecooled
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude oil was purified by column chromatography (0-0.5% MeOH-DCM)