反応 #89411

反応方程式

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

2-(tributylstannyl)pyrimidine

CsF

→

title compound

収率 67.2%

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

収率 67.2%

溶媒

DMF

反応条件

後処理

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

実験手順

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).

出典