HRID1685183

反应详情

EQUATION

反应方程式

HRID 1685183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine {2-[4-(4-fluoro-3-trifluoromethyl-phenyl)-2-piperidin-4-yl-imidazol-1-yl]-ethyl}-methyl-carbamic acid benzyl ester dihydrochloride (277 μmol; 160 mg); 4-chloro-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (1.30 equiv; 360 μmol; 61.1 mg); DMF (3 mL); TEA (7 equiv; 1.94 mmol; 270 μL) and heat to 160° C. in microwave for 45 min. Evaporate, dissolve the residue in DCM, wash with saturated sodium bicarbonate and evaporate the organic layer. Purify the residue on 40 g silica gel with 3% MeOH/DCM to provide the title compound (138.2 mg; 0.22 mmol; 78%). MS (ES+): m/z=638 (M+H).

WORKUP

后处理

  1. customEvaporate
  2. dissolutiondissolve the residue in DCM
  3. washwash with saturated sodium bicarbonate
  4. customevaporate the organic layer
  5. customPurify the residue on 40 g silica gel with 3% MeOH/DCM