HRID1661465

反应详情

EQUATION

反应方程式

HRID 1661465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 1-(4-fluorophenyl)-5-iodo-1H-indazole (0.224 g, 0.66 mmol), thiobenzoic acid (0.093 ml, 0.79 mmol), 3,4,7,8-tetramethyl-1,10-phenantroline (0.031 g, 0.13 mmol) and N,N-diisopropylamine (0.220 ml, 1.32 mmol) in toluene (2.5 ml) was added copper(I) iodine (2.245 μl, 0.07 mmol). The resulting mixture was stirred at 110C O/N. The reaction mixture was cooled to rt diluted with EtOAc and washed with water. The organic phase was the dried the solvent evaporated and then purified on HPLC. The relevant fractions were collected freeze dried to give 45 mg (20%) of product which was analysed by LC/MS.

WORKUP

后处理

  1. washwashed with water
  2. customdried the solvent
  3. customevaporated
  4. custompurified on HPLC
  5. customThe relevant fractions were collected freeze
  6. customdried