HRID879289

反应详情

EQUATION

反应方程式

HRID 879289 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

The reaction mixture of (S)-2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(3-(2-chloropyridin-4-yl)phenyl)-5-methylbenzo[d]thiazol-6-yl)ethyl pivalate (16 mg, 0.025 mmol), 1-methylpiperazine (1 mL) was heated at 120° C. overnight. Then the reaction mixture was washed by sat. NaHCO3, extracted by EtOAc, the organic phase was dried over MgSO4, filtered, concentrated. To the residue was added THF, MeOH, 2N NaOH, the mixture was heated at 45° C. After the reaction finished, the reaction was washed by sat NaHCO3, extracted by EtOAc, the organic phase was dried over MgSO4, filtered, concentrated down and purified by silica gel column, eluting by 0-100% EtOAc in hexanes to give the product. LCMS-ESI+: calc'd for C36H39ClN4O2S: 627.2 (M+H+); Found: 627.3 (M+H+).

WORKUP

后处理

  1. washThen the reaction mixture was washed by sat. NaHCO3
  2. extractionextracted by EtOAc
  3. dry with materialthe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. additionTo the residue was added THF, MeOH, 2N NaOH
  7. temperaturethe mixture was heated at 45° C
  8. washthe reaction was washed
  9. extractionextracted by EtOAc
  10. dry with materialthe organic phase was dried over MgSO4
  11. filtrationfiltered
  12. concentrationconcentrated down
  13. custompurified by silica gel column
  14. washeluting by 0-100% EtOAc in hexanes
  15. customto give the product