반응 #2275757

반응 방정식

N-({1-[4-(4-Iodo-pyrazol-1-yl)-cyclohexyl]-azetidin-3-ylcarbamoyl}-methyl)-3-trifluoromethyl-benzamide

TMS-acetylene

Et3N

→

title compound

3-Trifluoromethyl-N-({1-[4-(4-trimethylsilanylethynyl-pyrazol-1-yl)-cyclohexyl]-azetidin-3-ylcarbamoyl}-methyl)-benzamide

용매

DMF

반응 조건

후처리

1. 1
   기타The reaction was purified
2. 2
   기타column chromatography purification (0-100% ethyl acetate in hexanes with NH3 in MeOH)

실험 절차

A solution of N-({1-[4-(4-Iodo-pyrazol-1-yl)-cyclohexyl]-azetidin-3-ylcarbamoyl}-methyl)-3-trifluoromethyl-benzamide (as prepared in Example 28, 120 mg, 0.20 mmol), TMS-acetylene (Fluka, 20 mg, 0.40 mmol), Pd(Cl2)dppf (Aldrich, 16 mg, 0.02 mmol), CuI (Aldrich, 3.8 mg, 0.02 mmol) and Et3N (56 uL, 0.40 mmol) in DMF (5 mL) was heated to 80° C. overnight. The reaction was purified column chromatography purification (0-100% ethyl acetate in hexanes with NH3 in MeOH) resulting in the title compound as a white solid.

출처