2-Chloro-5-methoxy-4-nitro-benzoic acid methyl ester synthesis
- Product Name:2-Chloro-5-methoxy-4-nitro-benzoic acid methyl ester
- CAS Number:1349744-88-2
- Molecular formula:C9H8ClNO5
- Molecular Weight:245.62
67-56-1
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Yield:1349744-88-2 77%
Reaction Conditions:
with sulfuric acid for 18 h;Reflux;
Steps:
A54 Preparation of intermediate 350
Intermediate 349 (1.81 g, 4.69 mmol) was dissolved in MeOH (90 mL). Then, conc.H2S04 (1.81 mL) was added and the resulting mixture was heated under reflux for 18 h.Then, the reaction mixture was cooled down to rt, mixed with another batch (from 498mg of intermediate 349) and partitioned between water and EtOAc. The organic layerwas separated, dried over MgSO4, filtered and concentrated. The residue was purified by column chromatography on silica gel (irregular Si02, 80 g, mobile phase:heptane/EtOAc, 80:20). The fractions containing the products were mixed and the solvent was concentrated to afford 830 mg of intermediate 350 (77% yield).
References:
WO2017/125530,2017,A1 Location in patent:Page/Page column 290
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