反応 #3103

ord-89e91895296b44e384eadd8c11cead93

反応方程式

C1CCC2=NCCCN2CC1
1,8-diaza-bicyclo[5.4.0]undec-7-ene
CCOC(=O)CC(=O)c1ccc(OC)cc1
ethyl 3-(4-methoxyphenyl)-3-oxopropionate
O=[N+]([O-])C=Cc1ccc2c(c1)OCO2
3,4-methylenedioxy-1-(2-nitroethenyl)-benzene
CCOC(=O)C(C(=O)c1ccc(OC)cc1)C(C[N+](=O)[O-])c1ccc2c(c1)OCO2
Ethyl 2-(4-methoxybenzoyl)-3-(3,4-methylenedioxy-phenyl)-4-nitro-butanoate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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