反应 #861

ord-64d5f5dd2f664288acccc0452c5aa2a9

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After 6 hours of the reaction
  2. 2
    其他the product was purified by a silica gel column chromatography (eluent, chloroform/ethanol=1/2 containing 0.5% acetic acid)

实验过程

2.14 g (10.2 mmol) of 2-(2-aminoethoxy)ethyl benzoate and 0.624 g (10.4 mmol) of acetic acid were placed in a 50 ml two neck flask. While heating the flask in a 90° C. oil bath, 0.680 g (16.2 mmol) of cyanamide was added. After 6 hours of the reaction, the product was purified by a silica gel column chromatography (eluent, chloroform/ethanol=1/2 containing 0.5% acetic acid) to obtain 1.97 g of the title compound (wax-like, 6.33 mmol, 62.0% in yield) in the form of acetate. Results of the analysis of this compound are as follows.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723133uspto-grants-1998_03