HRID451197

反应详情

EQUATION

反应方程式

HRID 451197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-chloro-N-methyl-7-phenyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-amine (Preparation Gp) (26.0 mg, 100 μmol) in Dioxane (Ratio: 1, Volume: 175 μl) was added 4-(4-chloro-1H-imidazol-1-yl)-3-methoxyaniline (Preparation A) (22.37 mg, 100 μmol) and AcOH (Ratio: 1.000, Volume: 175 μl). The resulting mixture was brought to 100° C. and stirred overnight. The reaction mixture was brought to pH 10 by the addition of 1 N aqueous NaOH. The resulting mixture was extracted with EtOAc (3×4 mL). The combined organic extracts were washed with brine (4 mL), dried over MgSO4, filtered and concentrated in vacuo. The product was purified by Prep HPLC to yield the title compound. LC-MS (M+H)+=565.2.

WORKUP

后处理

  1. customwas brought to 100° C.
  2. extractionThe resulting mixture was extracted with EtOAc (3×4 mL)
  3. washThe combined organic extracts were washed with brine (4 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe product was purified by Prep HPLC