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ChemicalBook CAS DataBase List METHYL 3-METHOXY-2-NITROBENZOATE
5307-17-5

METHYL 3-METHOXY-2-NITROBENZOATE synthesis

10synthesis methods
-

Yield: 98%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide at 20; for 2 h;

Steps:

1.1 Step 1: Methyl 3-methoxy-2-nitrobenzoate (Compound c2)
To a mixture of 5 3-methoxy-2-nitrobenzoic acid (25.0 g, 126 mmol) and 6 K2CO3 (35.0 g, 253 mmol) in 7 DMF (126 mL) was added 8 MeI (15.8 mL, 253 mmol) at room temperature. The mixture was stirred at room temperature for 2 hours. To the mixture was poured the 9 water (200 mL) and then stirred at 5° C. for 30 min. The precipitated solid was collected by filtration, washed with water and hexane. The solid was dried under reduced pressure to afford the 10 title compound in a crude form (26.2 g, 98%) as a white solid. 1H NMR (400 MHz, CDCl3) δ 7.60 (dd, J=8.2, 1.2 Hz, 1H), 7.50 (t, J=8.2 Hz, 1H), 7.26 (dd, J=8.2, 1.2 Hz, 1H), 3.39 (s, 3H), 3.99 (s, 3H); [M+Na]+ 235.

References:

DAEWOONG PHARMACEUTICAL CO., LTD.;GREEN CROSS CORPORATION;YOON, Hee-kyoon;PARK, Se-Hwan;YOON, Ji-Sung;CHOI, Soongyu;SEO, Hee Jeong;PARK, Eun-Jung;KONG, Younggyu;SONG, Kwang-Seop;KIM, Min Ju;PARK, So Ok US2019/169174, 2019, A1 Location in patent:Paragraph 0259; 0260

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