反応 #5956

ord-b2cfaed8d84f496bad77a7ddcfae135c

反応方程式

S=C(NCCCN1CCN(c2ccccc2Cl)CC1)Nc1ccc2c(c1)OCCO2
N-3-[4-(2-chlorophenyl)piperazin-1-yl]propyl-N '-(3,4-ethylenedioxyphenyl)thiourea
c1ccc(P(c2ccccc2)c2ccccc2)cc1
triphenylphosphin
ClC(Cl)(Cl)Cl
carbon tetrachloride
CCN(CC)CC
triethylamine
Clc1ccccc1N1CCN(CCCN=C=Nc2ccc3c(c2)OCCO3)CC1
N-3-[4-(2-chlorophenyl)piperazin-1-yl]propyl-N'-(3,4-ethylenedioxyphenyl)carbodiimide
収率 56.5%

反応条件

温度
400°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction mixture was concentrated in vacuo
  2. 2
    ろ過The solution was filtered
  3. 3
    濃縮concentrated in vacuo

実験手順

A mixture of N-3-[4-(2-chlorophenyl)piperazin-1-yl]propyl-N '-(3,4-ethylenedioxyphenyl)thiourea of Example 11 (1.35 g; 3 mmol), triphenylphosphin (1.02 g; 3.9 mmol), carbon tetrachloride (0.56 ml), triethylamine (0.3 g; 3 mmol) and methylene chloride (15 ml) Was stirred at reflux for 3 h and at 400° C. for 16 h. The reaction mixture was concentrated in vacuo and then taken up in petroleum ether. The solution was filtered and concentrated in vacuo to give 0.7 g N-3-[4-(2-chlorophenyl)piperazin-1-yl]propyl-N'-(3,4-ethylenedioxyphenyl)carbodiimide as an oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05246935uspto-grants-1993_09