HRID1640990

反应详情

EQUATION

反应方程式

HRID 1640990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-[5-(3,5-difluoro-benzenesulfonyl)-1-trityl-1H-indazol-3-yl]-4-(4-methyl-piperazin-1-yl)-2-[(tetrahydro-pyran-4-yl)-(2,2,2-trifluoro-acetyl)-amino]-benzamide (2.4 g, 2.53 mmol), 4N hydrochloric acid in 1,4-dioxane (35 mL), methanol (50 mL) and 1,4-dioxane (15 mL) was stirred at room temperature for 3 hours. The solvents were removed under reduced pressure and the residue dissolved in dichloromethane, washed with water, brine, dried over sodium sulfate and evaporated to dryness. The crude was purified by flash chromatography on silica gel using dichloromethane/acetone 1:1 as the eluant affording the title compound as a pale yellow solid (1.43 g, 80% yield).

WORKUP

后处理

  1. customThe solvents were removed under reduced pressure
  2. dissolutionthe residue dissolved in dichloromethane
  3. washwashed with water, brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated to dryness
  6. customThe crude was purified by flash chromatography on silica gel