HRID28905

反应详情

EQUATION

反应方程式

HRID 28905 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To N′-(4-{4-(2-{3-[(dimethylamino)methyl]phenyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)-1-[2-(methylamino)ethyl]-1H-pyrazol-3-yl}phenyl)-N,N-dimethylurea.3TFA (300 mg, 0.34 mMol) in MeOH (10 mL) was added with stirring at RT, aq. 1 N NaOH and Ac2O (40 uL, 0.42 mMol). After stirring for 30 min. the reaction was diluted with water, basified with aq. 1 N NaOH (0.4 mL), extracted with (9:1) CHCl3/iPrOH, dried (Na2SO4), filtered, and evaporated to dryness under vacuum. Trituration with (1:1) Et2O and petroleum ether, filtration and drying under vacuum gave the title compound (177 mg, 90%) as an off-white solid. ESMS [M+H]+: 579.7.

WORKUP

后处理

  1. stirringAfter stirring for 30 min. the reaction
  2. extractionextracted with (9:1) CHCl3/iPrOH
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated to dryness under vacuum
  6. filtrationTrituration with (1:1) Et2O and petroleum ether, filtration
  7. customdrying under vacuum