HRID85450

反应详情

EQUATION

反应方程式

HRID 85450 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

To a 10-mL microwave tube were added methyl 6-bromo-1-(1-methylethyl)-1H-indazole-4-carboxylate (250 mg, 0.841 mmol), N,N-dimethyl-1-(4-piperidinyl)methanamine (132 mg, 0.925 mmol), Toluene (3 mL), and cesium carbonate (411 mg, 1.262 mmol), and the mixture was degassed for 5 min by bubbling N2 through BINAP (79 mg, 0.126 mmol) and Pd2(dba)3 (38.5 mg, 0.042 mmol) were added. The tube was sealed and the mixture was heated at 115° C. with stirring for 15 h. The mixture was diluted with methanol (5 mL) and filtered. The filtrate was concentrated and the residue was purified using reverse-phase HPLC to give 35 mg of product as a off-white solid. LCMS MH+=359.3

WORKUP

后处理

  1. customthe mixture was degassed for 5 min
  2. additionwere added
  3. customThe tube was sealed
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. customthe residue was purified