4-CHLORO-6-METHYL-NICOTINIC ACID METHYL ESTER synthesis
- Product Name:4-CHLORO-6-METHYL-NICOTINIC ACID METHYL ESTER
- CAS Number:886372-05-0
- Molecular formula:C8H8ClNO2
- Molecular Weight:185.61
67-56-1
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67367-33-3
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886372-05-0
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$75.00/100mg
Yield:886372-05-0 91%
Reaction Conditions:
Stage #1:4-hydroxy-6-methylnicotinic acid with trichlorophosphate for 2 h;Reflux;
Stage #2:methanol at 20;Cooling with ice;
Steps:
111 4-chloro-6-methylnicotinic acid methyl ester
3.26 g (19 mmol) of 4-hydroxy-6-methylnicotinic acid was dissolved in phosphorus oxychloride and refluxed for 2 hours,After cooling, the excess phosphorus oxychloride is distilled off. Ice bath,To the residue was added 30 mL of anhydrous methanol, and the mixture was stirred overnight at room temperature.The solvent was distilled off and diluted with water, extracted with ethyl acetate,The ethyl acetate layer was washed three times with brine and dried over anhydrous magnesium sulfate.The filtrate was concentrated on silica gel and flash column chromatography (0-20% ethyl acetate / petroleum ether) to give 3.23 g (91%) of a white solid.
References:
Shanghai Institute of Materia Medica, Chinese Academy of Sciences;Chen, Jianhua;Leng, Ying;Zhu, Junjie;Ning, Mengmeng CN103864754, 2016, B Location in patent:Paragraph 0655; 0656
67-56-1
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886372-05-0
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65973-52-6
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823-96-1
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886372-05-0
79 suppliers
$75.00/100mg
1005515-30-9
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886372-05-0
79 suppliers
$75.00/100mg
67-56-1
776 suppliers
$7.29/5ml-f
1060805-95-9
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886372-05-0
79 suppliers
$75.00/100mg