HRID1260043

反应详情

EQUATION

反应方程式

HRID 1260043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Methyl 2-diazo-7-methoxy-3-oxoheptanoate (6.93 g) and 1-phenylurea (5.41 g) were suspended in toluene (30 ml)-1,2-dichloroethane (30 ml), rhodium tetraacetate (230 mg) was added and the mixture was stirred at 80° C. for 2 hr. After cooling to room temperature, trifluoroacetic acid (7.5 ml) was added and the reaction mixture was stirred at room temperature for 1 day. The reaction mixture was concentrated under reduced pressure, and the residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (15:85-100:0) was concentrated under reduced pressure to give the object product (7.40 g).

WORKUP

后处理

  1. additionwas added
  2. temperatureAfter cooling to room temperature
  3. stirringthe reaction mixture was stirred at room temperature for 1 day
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. washa fraction eluted with ethyl acetate-hexane (15:85-100:0)
  6. concentrationwas concentrated under reduced pressure