4,6-Dichloronicotinic acid synthesis
- Product Name:4,6-Dichloronicotinic acid
- CAS Number:73027-79-9
- Molecular formula:C6H3Cl2NO2
- Molecular Weight:192
40296-46-6
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$6.00/1g
73027-79-9
269 suppliers
$13.00/1g
Yield:73027-79-9 96%
Reaction Conditions:
Stage #1: ethyl 4,6-dichloronicotinatewith sodium hydroxide;water in tetrahydrofuran;methanol; for 0.5 h;
Stage #2: with hydrogenchloride in tetrahydrofuran;methanol;water; pH=2;
Steps:
9.B
Sodium hydroxide (40 mL, 6.25 M solution) was added to a stirred solution of 4,6-dichloronicotinic acid ethyl ester (22) (25.95 g, 118 mmol) in 4:1:1 THF:MeOH:water (600 mL). After 30 minutes, the reaction mixture was acidified to pH 2 with concentrated HCl, diluted with 1:1 EtOAc:Et2O and washed with water and brine. The organic layer was dried (Na2SO4) and concentrated. The resulting off-white solid was twice concentrated from toluene to give the desired product (23) as a white solid (21.73 g, 96%).
References:
US2005/49419,2005,A1 Location in patent:Page/Page column 24
65973-52-6
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$6.00/1g
73027-79-9
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$13.00/1g
79-37-8
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$17.67/10gm:
5466-62-6
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$56.00/250mg
73027-79-9
269 suppliers
$13.00/1g
124-38-9
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$214.00/14L
343781-49-7
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$21.00/100mg
73027-79-9
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$13.00/1g
6975-44-6
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$17.67/250mgs:
73027-79-9
269 suppliers
$13.00/1g