3-cyano-2-methoxybenzoic acid synthesis
- Product Name:3-cyano-2-methoxybenzoic acid
- CAS Number:406938-74-7
- Molecular formula:C9H7NO3
- Molecular Weight:177.16
67-56-1
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124-41-4
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Yield:406938-74-7 94%
Reaction Conditions:
for 2 h;Reflux;Inert atmosphere;
Steps:
2.1 Step 1:
Tn a round-bottom flask 26 g (157.5 mmol) of 3-cyano-2-fluoro-benzoic acid was suspended in 315 mL (0.5 M) dry MeOH. To this suspension was added 144 mL (630 mmol) of NaOMe (25 wt% in MeOH). The resulting reaction mixture was refluxed for 2h underN2. After cooling to room temp., excess MeOH was evaporated under reduced pressure to obtain a thick slurry. To this slurry was added 158 mL (473 mmol) of 3 M aqueous HC1. The product precipitate as a white solid, which was isolated by filtration. The residual water was removed azeotropically using toluene to obtain 26.2 g (94%) of pure product.
References:
WO2018/136700,2018,A1 Location in patent:Paragraph 0275
406938-72-5
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406938-74-7
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