反応 #89410

反応方程式

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

5-chloro-2-iodobenzoic acid

DIPEA

HATU

→

title compound

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

溶媒

ethyl acetate

DMF

反応条件

後処理

1. 1
   洗浄washed with satd
2. 2
   その他The organic layer was separated
3. 3
   乾燥dried with MgSO4
4. 4
   濃縮concentrated in vacuo
5. 5
   その他The crude product was purified by chromatography on silica gel (EtOAc/hex)

実験手順

A mixture of 2-(((2S,3R)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione (0.70 g, 2.71 mmol), 5-chloro-2-iodobenzoic acid (0.66 g, 2.32 mmol), DIPEA (1.21 mL, 6.97 mmol) and HATU (1.06 g, 2.79 mmol) in DMF (5 ml) was stirred at rt for 1 h. The reaction mixture was diluted with ethyl acetate and washed with satd. aq. NaHCO3 and brine successively. The organic layer was separated, dried with MgSO4 and concentrated in vacuo. The crude product was purified by chromatography on silica gel (EtOAc/hex) to afford the title compound. MS (ESI) 523 (M+H).

出典