HRID79371

反应详情

EQUATION

反应方程式

HRID 79371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3-(chloromethyl)-1,5-dimethyl-1H-pyrazole hydrochloride (5.01 g, 27.7 mmol) in DMF (50 mL) was added 3-iodo-4-nitro-1H-indazole (8.00 g, 27.7 mmol) and K2CO3 (15.3 g, 111 mmol). The reaction mixture was stirred for 20 hours. The mixture was concentrated under reduced pressure to remove most of the DMF. The residue was diluted with DCM (100 mL) and washed with H2O. The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by silica gel chromatography (EtOAc/Hexane 1:3) to provide the product (8.35 g).

WORKUP

后处理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customto remove most of the DMF
  3. additionThe residue was diluted with DCM (100 mL)
  4. washwashed with H2O
  5. dry with materialThe organic phase was dried (Na2SO4)
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (EtOAc/Hexane 1:3)