HRID244686

反应详情

EQUATION

反应方程式

HRID 244686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(1-Methylethyl)-1H-pyrazole-5-carbonyl chloride (152 mg) in DCM (10 ml) was added dropwise to 1-(phenylsulfonyl)-6-(trimethylstannanyl)-1H-indazol-4-amine (350 mg) in DCM (15 ml) and pyridine (0.07 ml). The reaction was stirred at room temperature for 10 min before addition of further 1-(1-methylethyl)-1H-pyrazole-5-carbonyl chloride (10 mg). The reaction was stirred for 30 min, saturated sodium bicarbonate (aq) (25 ml) was added and stirred vigorously for 10 min before the DCM was separated through a hydrophobic frit and evaporated to dryness. The residue was dissolved in DCM and loaded onto a silica cartridge preconditioned with cyclohexane. The cartridge was eluted with 0-100% ether in cyclohexane. The compound containing fraction was evaporated to dryness to give title compound, 360 mg.

WORKUP

后处理

  1. customwas separated through a hydrophobic frit
  2. customevaporated to dryness
  3. dissolutionThe residue was dissolved in DCM
  4. washThe cartridge was eluted with 0-100% ether in cyclohexane
  5. additionThe compound containing fraction
  6. customwas evaporated to dryness