반응 #87519

반응 방정식

methyl iodide

2-methoxy-5-nitrobenzoic acid

K2CO3

→

desired product

수율 78.9%

methyl 2-methoxy-5-nitrobenzoate

수율 78.9%

용매

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGThe reaction mass was further stirred at 80° C. for 5-6 h
2. 2
   여과The reaction mass was filtered
3. 3
   농축the obtained filtrate was concentrated
4. 4
   workup.ADDITIONThe residue was further diluted with water
5. 5
   기타obtained solid
6. 6
   여과was filtered off

실험 절차

To a solution of 2-methoxy-5-nitrobenzoic acid (25.0 g, 0.12 mol) in DMF (100 mL) was added K2CO3 (26.3 g, 0.19 mol). The reaction mass was stirred at 80° C. for 1 h followed by addition of methyl iodide (12.3 mL, 0.19 mol). The reaction mass was further stirred at 80° C. for 5-6 h. The reaction mass was filtered and the obtained filtrate was concentrated. The residue was further diluted with water and obtained solid was filtered off to afford 20.0 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 3.83 (s, 3H), 3.97 (s, 3H), 7.38 (d, 0.1=9.3 Hz, 1H), 8.41 (dd, J=2.4 Hz & 2.4 Hz, 1H), 8.47 (s, 1H); MS (m/z): 212.44 (M+H)+.

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