HRID1928374

反应详情

EQUATION

反应方程式

HRID 1928374 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The title compound was prepared from the above described 3-[6′-methyl-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-benzenesulfonic acid 2,2-dimethyl-propyl ester (7.7 g, 14.24 mmol) by refluxing in 1-propanol (15 mL) with sodium propanolate (1.7 M in n-propanol, 20.95 ml, 35.6 mmol) and 2-(diethylamino)ethanthiol (2.48 mL, 16.38 mmol) for 18 h. Cooled to rt, added water (300 mL), added 1 N HCl (ca. 50 mL) until pH 3-4 was reached, stirred for 10 min, filtered the solid off, washed thrice with water, and then with acetone and dried in HV to give the title compound (5.4 g, 81%) as an off-white solid. MS (ISN) 469.1 [(M−H)−].

WORKUP

后处理

  1. customThe title compound was prepared from the
  2. filtrationfiltered the solid off,
  3. washwashed thrice with water
  4. dry with materialwith acetone and dried in HV