HRID410120

反应详情

EQUATION

反应方程式

HRID 410120 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-(3-chloro-4-fluoro-phenyl)-2-{2,6-dichloro-3-[(tert-butoxy-carbonylamino)-methyl]phenylamino}-6-(2,2-difluoroethoxy)-1-methyl-1H-benzimidazole-5-carboxylic acid amide (4.0 g, 5.9 mmol, prepared in analogy to example 75 from N-(3-chloro-4-fluorophenyl)-2-(2,2-difluoroethoxy)-4-methylamino-5-amino-benzamide with building block B), 4 M HCl in dioxane (50 mL) and dioxane (200 mL) is stirred for 2 h. The precipitate is filtered off, washed with water and diluted with 10 mL conc. aq. NH3. The mixture is extracted with EtOAc, the organic phase is dried with Na2SO4 and concentrated.

WORKUP

后处理

  1. filtrationThe precipitate is filtered off
  2. washwashed with water
  3. additiondiluted with 10 mL conc. aq. NH3
  4. extractionThe mixture is extracted with EtOAc
  5. dry with materialthe organic phase is dried with Na2SO4
  6. concentrationconcentrated