HRID571894

反应详情

EQUATION

反应方程式

HRID 571894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of N-[5-(3,5-Difluoro-benzoyl)-1-trityl-1H-indazol-3-yl]-4-(4-methyl-piperazin-1-yl)-2-nitro-benzamide (2.76 g, 3.62 mmol), trifluoroacetic acid (5.6 mL) and dichloromethane (56 mL) was stirred at room temperature for 2 hours. The volatiles were evaporated and the residue taken up with dichloromethane and washed with a saturated solution of sodium hydrogen-carbonate. The organic phase was evaporated to dryness. The residue was redissolved in ethyl acetate and washed twice with brine. The resulting organic phase was dried over sodium sulfate and evaporated to dryness. Purification of the crude by chromatography over silica gel (DCM/MeOH) and trituration of the so obtained compound from diethyl ether afforded 1.47 g of the title compound (78% yield).

WORKUP

后处理

  1. customThe volatiles were evaporated
  2. washwashed with a saturated solution of sodium hydrogen-carbonate
  3. customThe organic phase was evaporated to dryness
  4. dissolutionThe residue was redissolved in ethyl acetate
  5. washwashed twice with brine
  6. dry with materialThe resulting organic phase was dried over sodium sulfate
  7. customevaporated to dryness
  8. customPurification of the crude by chromatography over silica gel (DCM/MeOH) and trituration of the so obtained compound from diethyl ether