HRID544560

反应详情

EQUATION

反应方程式

HRID 544560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution (2.75 ml.) of bromine (80 mg.) in chloroform was added to a solution of 1-(4-hydroxybutyl)-3-[2-(2,2,2-trifluoroethyl)guanidino]pyrazole (140 mg.) in HOAc (2 ml.). After stirring at room temperature for 1 hour the mixture was basified with 6 N aqueous ammonium hydroxide and then extracted with EtOAc (6×10 ml.). The combined extracts were dried (MgSO4) and evaporated to dryness in vacuo to give 4-bromo-1-(4-hydroxybutyl)-3-[2-(2,2,2-trifluoroethyl)guanidino]pyrazole (145 mg., 82%) having the following n.m.r. spectrum in d6DMSO: 7.7 (s, 1H); 4.2 (br t, 2H); 3.9 (t, 2H); 3.3 (t, 2H); 1.5 (br m, 4H).

WORKUP

后处理

  1. extractionextracted with EtOAc (6×10 ml.)
  2. dry with materialThe combined extracts were dried (MgSO4)
  3. customevaporated to dryness in vacuo