4-Bromo-2,5-dimethoxybenzaldehyde synthesis
- Product Name:4-Bromo-2,5-dimethoxybenzaldehyde
- CAS Number:31558-41-5
- Molecular formula:C9H9BrO3
- Molecular Weight:245.07
25245-34-5
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1191-17-9
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31558-41-5
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Yield:31558-41-5 87%
Reaction Conditions:
with titanium tetrachloride in dichloromethane at -78; for 1 h;
Steps:
1
2,5-Dimethoxybromobenzene (5) (7.0 ml :47 mmol) was dissolved in 160 ml of dichloromethane. The solution was added with 13 ml (0.12 mol) of titanium chloride (IV) under argon atmosphere at -78°C, subsequently with 8.2 ml (0.14 mol ) of dichloromethylmethy ether, and stirred at -78°C for one hour. The reaction mixture was gradually added to 600 ml of ice water and extracted with dichloromethane. The dichloromethane layer was washed with an aqueous saturated sodium hydrogencarbonate solution, water, and saturated brine, and then dried over sodium sulfate. The dichloromethane was evaporated under reduced pressure, and the residue was purified by silica gel column to obtain 9.9 g of Compound (6) (yield 87 %).1H-NMR (CDCl3, 300 MHz): 10.40 (s, 1H), 7.34 (s, 1H), 7.25 (s, 1H), 3.91 (s, 3H), 3.90 (s, 3H)
References:
Daiichi Pure Chemicals Co. Ltd.;Nagano, Tetsuo EP1403268, 2004, A1 Location in patent:Page 10
93-02-7
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31558-41-5
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$7.00/250mg
4885-02-3
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25245-34-5
239 suppliers
$8.00/5g
31558-41-5
112 suppliers
$7.00/250mg
72054-76-3
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31558-41-5
112 suppliers
$7.00/250mg