反应 #3103

ord-89e91895296b44e384eadd8c11cead93

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The reaction mixture was filtered through dicalite
  2. 2
    过滤the resulting filtered solution
  3. 3
    其他was used in the next step without any further purification

实验过程

Into a 45-L stirred reactor at ambient temperature were charged 5.819 kg (30.1 moles) 3,4-methylenedioxy-1-(2-nitroethenyl)-benzene and 24 L ethyl acetate. A solution of 5.355 kg (24.1 moles) ethyl 3-(4-methoxyphenyl)-3-oxopropionate in 16 L ethyl acetate was added. 280 g (275 ml, 1.84 moles) of 1,8-diaza-bicyclo[5.4.0]undec-7-ene in four equal portions was added over a 2.5 hour period. The reaction mixture was filtered through dicalite and the resulting filtered solution was used in the next step without any further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05731434uspto-grants-1998_03