HRID747123

反应详情

EQUATION

反应方程式

HRID 747123 的结构方程式

PROCEDURE

实验过程

Analogous to the procedure used to prepare Example 5(b), 4-chloro-6-(4-trifluoromethylphenyl)pyrimidine, Example 5(a), (200 mg, 0.77 mmol) and 3-methylsulphonylaniline hydrochloride (80 mg, 0.39 mmol, Acros) afforded a crude reaction product mixture, which was partitioned between EtOAc (100 mL) and 1 N NaOH (50 mL). The organic layer was washed with 1 N NaOH (50 mL), water (50 mL), satd NaCl (20 mL), dried over Na2SO4, filtered and concentrated in vacuo. Purification by silica gel chromatography (9:1 CH2Cl2/EtOAc) provided the title product as a white solid. MS (ESI, pos. ion) m/z: 394 (M+1). MP: 204-205° C.

WORKUP

后处理

  1. customafforded a crude
  2. customreaction product mixture, which
  3. customwas partitioned between EtOAc (100 mL) and 1 N NaOH (50 mL)
  4. washThe organic layer was washed with 1 N NaOH (50 mL), water (50 mL), satd NaCl (20 mL)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customPurification by silica gel chromatography (9:1 CH2Cl2/EtOAc)