반응 #89411

반응 방정식

2-(((2S,3R)-1-(5-chloro-2-iodobenzoyl)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione

2-(tributylstannyl)pyrimidine

CsF

→

title compound

수율 67.2%

2-(((2S,3R)-1-(5-Chloro-2-(pyrimidin-2-yl)benzoyl)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione

수율 67.2%

용매

DMF

반응 조건

후처리

1. 1
   기타was degassed
2. 2
   기타The solvent was removed in vacuo
3. 3
   기타to obtain the crude which
4. 4
   기타was purified by silica gel chromatography (0˜100% EtOAc/hexanes)

실험 절차

A mixture of 2-(((2S,3R)-1-(5-chloro-2-iodobenzoyl)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione (0.22 g, 0.42 mmol), 2-(tributylstannyl)pyrimidine (0.16 ml, 0.51 mmol), CsF (128 mg, 0.84 mmol), CuI (16 mg, 0.08 mmol) and Pd(PPh3)4 (49 mg, 0.04 mmol) in DMF (5 mL) was degassed and heated at 120° C. for 1 h in a microwave reactor. The solvent was removed in vacuo to obtain the crude which was purified by silica gel chromatography (0˜100% EtOAc/hexanes) to yield the title compound as a white solid (0.134 g, 67%). MS (ESI) 475 (M+H).

출처