3,5-Dimethoxybenzoic acid synthesis
- Product Name:3,5-Dimethoxybenzoic acid
- CAS Number:1132-21-4
- Molecular formula:C9H10O4
- Molecular Weight:182.17
Yield:1132-21-4 98%
Reaction Conditions:
with potassium carbonate in acetone at 55;
Steps:
1.1 (1) Preparation of intermediate 2 (ie compound 2): 3,5-dimethoxybenzoic acid
Add to 100mL single-mouth flask3,5-dihydroxybenzoic acid (1.54 g, 10 mmol),Dissolve it by adding 20 mL of acetone.Potassium carbonate (4.14 g, 30 mmol) was added at room temperature.At the same time, 3.5 mL of dimethyl sulfate was added dropwise.Heated to 55 ° C,The reaction was refluxed overnight.After the reaction is complete,Concentrate and recover acetone under reduced pressure.Add 30mL of water,Then add a 30% sodium hydroxide solution to adjust the pH to 14,React at 75 ° C for 4 hours,After the hydrolysis is complete, the system is cooled to room temperature.Adjust the pH to about 6 with concentrated hydrochloric acid.There are a lot of white solids,Filtered,Washed,The title compound 2 (1.78 g, yield 98%) was obtained.
References:
Southeast University;Cai Jin;Liu Wenjing;Ji Min;Wang Yingying;Ning Yao;Mai Dinuer·tuerxun;Xu Hongqin CN108484510, 2018, A Location in patent:Paragraph 0041
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