HRID563526

反应详情

EQUATION

反应方程式

HRID 563526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

[2′-(3-Cyano-1-ethyl-2-phenyl-isoureidomethyl)-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl]-acetic acid ethyl ester (0.10 g, 0.17 mmol) and benzylamine (0.04 mL, 0.34 mmol) were combined in EtOH (1 mL) and heated to 60° C. The reaction was monitored by analytical LCMS, and additional benzylamine (0.04 mL, 0.34 mmol) was added to push the reaction to completion. Further benzylamine (0.10 mL, 0.92 mmol) was added, and the reaction was heated for a total of 48 hours. The mixture was partitioned between EtOAc and H2O, and the aqueous layer was extracted with EtOAc. The combined organic layers were concentrated and purified by silica gel chromatography (0-50% EtOAc in hexanes) to give the title compound.

WORKUP

后处理

  1. additionwas added
  2. customthe reaction to completion
  3. temperaturethe reaction was heated for a total of 48 hours
  4. customThe mixture was partitioned between EtOAc and H2O
  5. extractionthe aqueous layer was extracted with EtOAc
  6. concentrationThe combined organic layers were concentrated
  7. custompurified by silica gel chromatography (0-50% EtOAc in hexanes)