反応 #162112

反応方程式

5-chloro-3-(5-fluoro-4-methylsulfinyl-pyrimidin-2-yl)-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridine

(1S,2S)-cyclohexane-1,2-diamine

iPr2NEt

→

desired intermediate

(1S,2S)—N1-(2-(5-chloro-1-tosyl-1H-pyrrolo[2,3-b]pyridin-3-yl)-5-fluoropyrimidin-4-yl)cyclohexane-1,2-diamine

溶媒

THF

反応条件

後処理

1. 1
   濃縮The mixture was concentrated in vacuo
2. 2
   その他The resulting residue was purified by silica gel chromatography (0-20% MeOH—CH2Cl2)

実験手順

A solution of 5-chloro-3-(5-fluoro-4-methylsulfinyl-pyrimidin-2-yl)-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridine, 23a, (0.50 g, 1.08 mmol) in THF (4 mL) was treated with (1S,2S)-cyclohexane-1,2-diamine (0.27 g, 2.37 mmol) and iPr2NEt (2.15 mmol) at 120° C. for 10 minutes. The mixture was concentrated in vacuo. The resulting residue was purified by silica gel chromatography (0-20% MeOH—CH2Cl2) to provide the desired intermediate as a white solid (410 mg).

出典