HRID1760979

反应详情

EQUATION

反应方程式

HRID 1760979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of N-(3-amino-4-methylphenyl)dibenzofuran-4-carboxamide (1.5 g), 2,4-dichloropyrimidine (1.4 g), N,N-di-isopropylethylamine (2.9 ml) and n-butanol (70 ml) was stirred and heated to 120° C. for 76 hours. The mixture was evaporated and the residue was purified by column chromatography on silica using increasingly polar mixtures of isohexane and ethyl acetate as eluent. The material so obtained was triturated under ethyl acetate. There was thus obtained the title compound (0.83 g); NMR Spectrum: (DMSOd6) 2.17 (s, 3H), 6.53 (d, 1H), 7.31 (d, 1H), 7.43-7.65 (m, 4H), 7.79 (m, 2H), 7.84 (d, 1H), 8.1 (d, 1H), 8.21 (d, 1H), 8.34 (d, 1H), 9.62 (s, 1H), 10.42 (s, 1H); Mass Spectrum: M+H+ 429 and 431.

WORKUP

后处理

  1. customThe mixture was evaporated
  2. customthe residue was purified by column chromatography on silica using
  3. temperatureincreasingly polar mixtures of isohexane and ethyl acetate as eluent
  4. customThe material so obtained
  5. customwas triturated under ethyl acetate