HRID1927987

反应详情

EQUATION

反应方程式

HRID 1927987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 3-{4-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyrimidin-2-yl]-pyridin-2-yl}-benzenesulfonic acid 2,2-dimethyl-propyl ester (1.27 g, 2.13 mmol), 37% HCl (12.5 ml) and dioxane (12.5 ml) was heated under reflux conditions for 19 h and evaporated to dryness. Diethyl ether (50 ml) was added to the crude product and the mixture was stirred at room temperature for 1 h. The precipitate was collected by filtration and dried to yield 3-{4-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyrimidin-2-yl]-pyridin-2-yl}-benzenesulfonic acid hydrochloride as a white solid (1.08 g, 90%). MS (ISN) 524.0 [(M−H)−]; mp 407° C. (dec.).

WORKUP

后处理

  1. temperaturewas heated under reflux conditions for 19 h
  2. customevaporated to dryness
  3. additionDiethyl ether (50 ml) was added to the crude product
  4. filtrationThe precipitate was collected by filtration
  5. customdried