HRID1266899

反应详情

EQUATION

反应方程式

HRID 1266899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of (2-amino-5-methyl-4-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester (Example J15) (0.145 g) and 3-oxo-3-[3-[4-(tetrahydro-pyran-2-yloxymethyl)-thiazol-2-yl]-phenyl]-propionic acid tert.-butyl ester (Example K19) (0.23 g) in toluene (2 mL) was heated to 100° C. for 5 h. The mixture was cooled and evaporated in vacuum. A solution of the residue in a mixture of CH2Cl2 (2 mL) and TFA (2 mL) was stirred for 0.5 h at 20° C. The mixture was evaporated in vacuum, the residual oil was dissolved in AcOEt and the solution was washed with saturated NaHCO3 solution and with brine, dried over Na2SO4 and evaporated in vacuum. The residue was crystallized from CH2Cl2/hexane to give the title compound (0.04 g) as light-brown crystals.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. customevaporated in vacuum
  3. additionA solution of the residue in a mixture of CH2Cl2 (2 mL) and TFA (2 mL)
  4. customThe mixture was evaporated in vacuum
  5. dissolutionthe residual oil was dissolved in AcOEt
  6. washthe solution was washed with saturated NaHCO3 solution and with brine
  7. dry with materialdried over Na2SO4
  8. customevaporated in vacuum
  9. customThe residue was crystallized from CH2Cl2/hexane