2-chloro-3,4-dihydroxybenzaldehyde synthesis
- Product Name:2-chloro-3,4-dihydroxybenzaldehyde
- CAS Number:32864-11-2
- Molecular formula:C7H5ClO3
- Molecular Weight:172.57
37687-57-3
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Yield: 94.8%
Reaction Conditions:
Stage #1:2-chloro-3-hydroxy-4-methoxybenzaldehyde with boron tribromide in dichloromethane at -20.5 - 26; for 2 h;
Stage #2: with hydrogenchloride in methanol;dichloromethane;water; pH=3 - 4 at -5 - 60; for 3.5 h;Temperature;pH-value;
Steps:
1-10
Add 3g (0.016mol) 2-chloro-4-methoxy-3-hydroxybenzaldehyde to a 250ml three-necked flask, add 35ml dichloromethane, stir to dissolve, add 6g (0.024mol) BBr3 dropwise at -20.5°C, After the addition is complete, place the reaction solution at room temperature and stir for 2 hours. In an ice-water bath environment (-5°C), slowly add 75ml of methanol dropwise. After 1.5h, place at room temperature (26°C) and use 20ml of aqueous hydrochloric acid (25%). ) Adjust the pH of the reaction solution to 3~4, heat to reflux, the temperature is 60°C, the reflux time is 2h, and filter to obtain 2.61g of brown solid product, the yield is 94.8%, and the purity is 95.7%.
References:
CN112390711, 2021, A Location in patent:Paragraph 0014-0024
5417-17-4
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![Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-](/CAS/20210305/GIF/1000210-73-0.gif)