반응 #89338

반응 방정식

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

2-iodo-5-methylbenzoic acid

DIPEA

HATU

→

title compound

2-(((2S,3R)-1-(2-Iodo-5-methylbenzoyl)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione

용매

ethyl acetate

DMF

반응 조건

후처리

1. 1
   세척washed with satd
2. 2
   기타The organic layer was separated
3. 3
   건조dried with MgSO4
4. 4
   농축concentrated in vacuo
5. 5
   기타The crude product was purified by chromatography on silica gel (EtOAc/hexanes)

실험 절차

A mixture of 2-(((2S,3R)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione (0.70 g, 2.71 mmol), 2-iodo-5-methylbenzoic acid (0.64 g, 2.71 mmol), DIPEA (1.41 mL, 8.13 mmol) and HATU (1.24 g, 3.25 mmol) in DMF (4 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/hexanes) to afford the title compound. MS (ESI) 503 (M+H).

출처