4-ISOBUTOXY-3-METHOXYBENZALDEHYDE synthesis
- Product Name:4-ISOBUTOXY-3-METHOXYBENZALDEHYDE
- CAS Number:66488-79-7
- Molecular formula:C12H16O3
- Molecular Weight:208.25
Yield:-
Reaction Conditions:
with potassium carbonate in N,N-dimethyl-formamide; for 20 h;Inert atmosphere;Reflux;
Steps:
12.1 1).
Synthesis of 4-(2-methylpropyloxy)-3-methoxybenzaldehyde.
1).
Synthesis of 4-(2-methylpropyloxy)-3-methoxybenzaldehyde.
In 250 ml three necked flask, equipped with reflux condenser, mechanical stirrer, 30.4 g (200 mmol) of vanillin, 28 g (200 mmol) of dry K2CO3 and 150 ml of abs.
dimethylformamide are placed in the flow of argon.
The mixture is stirred for 20 min in argon condition, then 34.3 g (250 mmol) of isobutyl bromide is added.
The mixture is refluxed with stirring in argon condition for 20 h at 90÷100° C., and concentrated in vacuum at 50÷80° C. to dryness.
Then 200 ml of water is added to the residue, the mixture is extracted with (4*100 ml) of dichloromethane.
The combined organic fraction is washed with 7% NaOH solution, dried over magnesium sulfate, filtered off, concentrated in vacuum at 50÷80° C.
The residue (15 g of brown oil)-crude 4-(2-methylpropyloxy)-3-methoxybenzaldehyde is used on the next step without further purification.
References:
US2013/267707,2013,A1 Location in patent:Paragraph 0150; 0151
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