HRID2190660

反应详情

EQUATION

反应方程式

HRID 2190660 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-iodo-4-methyl-phenyl)-6-piperazin-1-yl-nicotinamide (60 mg, 0.14 mmol), trans-1,4-cyclohexane dicarboxylic acid (122 mg, 0.71 mmol) in DMF (10 mL) was treated with EDCI (130 mg, 0.71 mmol). After stirring overnight the reaction mixture was partitioned between EtOAc and water. The water layer was made basic to pH 13 with solid NaOH. The EtOAc layer was removed and then the water layer was acidified to pH 5 with aq conc. HCl and extracted again with EtOAc. The EtOAc layer obtained after the latter extraction was dried over Na2SO4, filtered and concentrated to the product (10 mg, Yield: 12%). HRMS m/z calcd for C25H29N4O4I [M+H]+: 577.1306. Found: 577.1306.

WORKUP

后处理

  1. customwas partitioned between EtOAc and water
  2. customThe EtOAc layer was removed
  3. extractionextracted again with EtOAc
  4. customThe EtOAc layer obtained
  5. extractionafter the latter extraction
  6. dry with materialwas dried over Na2SO4
  7. filtrationfiltered