2,4-Dichloro-5-methoxybenzoic acid synthesis
- Product Name:2,4-Dichloro-5-methoxybenzoic acid
- CAS Number:71685-44-4
- Molecular formula:C8H6Cl2O3
- Molecular Weight:221.04
67-56-1
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71685-44-4
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Yield:71685-44-4 100%
Reaction Conditions:
with sodium hydride in N,N-dimethyl-formamide at 120; for 12 h;Cooling with ice;
Steps:
70
Reference Example-70
2,4-Dichloro-5-fluorobenzoic acid (25.0 g, 118 mmol), and methanol (5.4 mL, 134 mmol) were added to a suspension of a 55% oil dispersion (10.33 g, 237 mmol) of sodium hydride in DMF (250 mL) under ice-cooling, followed by stirring at 120° C. for 12 hours.
After the reaction was completed, the reaction solution was cooled to room temperature, and concentrated hydrochloric acid was added until the reaction solution became acidic, and the resultant product was extracted with diethyl ether (100 mL*3).
The combined organic layer was washed with water, dried over magnesium sulfate, concentrated under reduced pressure, and dried under reduced pressure, whereby 2,4-dichloro-5-methoxybenzoic acid (quantitative) was obtained as a pale gray solid. 1H-NMR (400 MHz, CDCl3): δ3.96 (s, 3H), 7.52 (s, 1H), 7.58 (s, 1H).
References:
US2016/24110,2016,A1 Location in patent:Paragraph 1102; 1103
725246-15-1
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71685-44-4
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$200.00/0.5g