4-Amino-2-methyl-benzaldehyde synthesis
- Product Name:4-Amino-2-methyl-benzaldehyde
- CAS Number:61594-81-8
- Molecular formula:C8H9NO
- Molecular Weight:135.16
Yield:61594-81-8 87 %
Reaction Conditions:
Stage #1: ethanolwith trichlorophosphate at 0 - 5;Inert atmosphere;
Stage #2: 1-amino-3-methylbenzene at 0 - 65;Inert atmosphere;
Steps:
2
Under nitrogen protection, 600 mL of DMF was added to a 2L three-necked flask.Control the temperature at 0-5° C., and add 343 g of phosphorus oxychloride dropwise to the above system.After the dropwise addition, stirring was continued at 0-5°C for 1 hour.Control the temperature at 0-5°C, and add 1200g of the compound in batches.When the addition is complete, the cold pump is removed.Raise the temperature to 60-65°C and keep it warm for 5-6 hours. TLC (PE:EA=3:1) detects until the raw material disappears.Let cool to room temperature.The temperature was controlled at 0-5°C, and the above system was poured into 2L of ice water with stirring.Adjust the pH to 8-9 with 10% sodium hydroxide.Filter and wash the filter cake with water to obtain a yellow solid.Vacuum drying at 40°C for 8 hours yielded 220 g of a yellow solid with a yield of 87% and a purity of 99.5%.
References:
CN115304472,2022,A Location in patent:Paragraph 0034-0037
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