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CAS No. : | 49668-99-7 | MDL No. : | MFCD09878512 |
Formula : | C9H10ClNO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 199.63 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Danger | Class: | 8 |
Precautionary Statements: | P264-P270-P271-P280-P303+P361+P353-P304+P340-P305+P351+P338-P310-P330-P331-P363-P403+P233-P501 | UN#: | 3261 |
Hazard Statements: | H302-H314 | Packing Group: | Ⅱ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | With thionyl chloride | |
100% | With thionyl chloride In dichloromethane at 0℃; for 1.5h; | A001.2 Thoroughly dried 6-(hydroxymethyl) pyridine-2-carboxylic acid ethyl ester (28 g, 154 mmol) was dissolved in DCM (400 mL) was added dropwise of 50C12 (56 mL) at 0°C. After 90 mm the solution was allowed to reach room temperature and the excess of 50C12 was removedunder reduced pressure without heating. DCM (500 mL) was added to the oily residue, and the solution was washed with saturated aqueous of NaHCO3 and dried over Na2504. Evaporation of the solvent afforded 2-(chloromethyl)pyridine-6-carboxylic acid ethyl ester (31 g in 100% yield) as an orange oil. ‘H NMR (DMSO-d6) 8.0 1-8.08 (m, 2H), 7.81 (d, 1H, J=7.2 Hz), 4.86 (s, 2H), 4.37 (q, 2H, J=6.0 Hz), 1.34 (t, 3H, J=7.2 Hz). |
96% | With thionyl chloride at 0℃; for 1h; |
96% | With thionyl chloride at 0℃; | |
91% | With thionyl chloride; sodium carbonate In water | |
85.6% | With thionyl chloride at 0 - 20℃; for 18h; | |
83% | With thionyl chloride at 0℃; for 1.5h; | |
With thionyl chloride In chloroform at 20℃; for 1h; | ||
With thionyl chloride In dichloromethane at 10 - 20℃; for 1.25h; | 3 Ethyl 6-(chloromethyl)-2-pyridinecarboxylate; Thionyl chloride (13.8ml) was added over - 15 minutes to a stirred solution of ethyl 6- (hydroxymethyl)-2-pyridinecarboxylate (28.5g) in MDC (200ml) maintaining the temperature at 10-150C using an ice-water bath. On completion of the addition the mixture was stirred at room temperature for 1 hour. The solvent was evaporated and the residue partitioned between toluene (200ml)/saturated bicarb (sodium bicarbonate solution, 200ml). The layers were separated and the organic phase washed with water (150ml). The solvent was evaporated to leave a pale oil which solidified on standing. (31.3g). | |
29.5 g | With thionyl chloride In dichloromethane at 10 - 25℃; for 1h; | |
With thionyl chloride In dichloromethane | ||
With thionyl chloride In dichloromethane at 20℃; for 5.5h; Cooling with ice; | 1.2 synthesis of ethyl 6-chloromethyl-2-pyridinecarboxylate 1.81 g of ethyl 6-hydroxymethyl-2-formate pyridine and 730 yL of thionyl chloride were added to a round bottom flask containing 28 mL of dry methylene chloride, 6-hydroxymethyl-2-formylpyridine and The molar ratio of thionyl chloride was 1: 1, stirred for 30 min on an ice bath, and then stirred at room temperature for 5 h. After the completion of the reaction, the methylene chloride was evaporated to dryness, and the toluene was dissolved. The organic layer was washed with water (0.1 m? / L sodium hydrogencarbonate solution) and then the organic layer was washed with water, dried over anhydrous sodium sulfate and evaporated to remove 6- Chloromethyl-2-carboxylate pyridine. | |
Stage #1: ethyl 6-(hydroxymethyl)pyridine-2-carboxylate With thionyl chloride In dichloromethane at 10 - 20℃; for 1.25h; Stage #2: With sodium hydrogencarbonate In water; toluene | 1.b Step (b) Ethyl 6-(chloromethyl)-2-pyridinecarboxylate; Thionyl chloride (13.8ml) was added over - 15 minutes to a stirred solution of ethyl 6- (hydroxymethyl)-2-pyridinecarboxylate (28.5g) in MDC (200ml) maintaining the temperature at 10-150C using an ice-water bath. On completion of the addition the mixture was stirred at room temperature for 1 hour. The solvent was evaporated and the residue partitioned between toluene (200ml)/saturated bicarb (sodium bicarbonate solution, 200ml) The layers were separated and the organic phase washed with water (150ml). The solvent was evaporated to leave a pale oil which solidified on standing (31.3g). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate;tetrakis(triphenylphosphine) palladium(0); In ethanol; toluene; at 90℃; for 3h; | Description 5 Ethyl 6-[5-chloro-2-(methyloxy)phenyl]methyl}-2-pyridinecarboxylate (D5) <n="35"/>A mixture of delta-chloro^-methoxyphenylboronic acid (2.33g, 12.5mmol), methyl 6- (chloromethyl)-2-pyridinecarboxylate (2.32g, 12.5mmol), potassium carbonate (6.9g, 50mmol) and tetrakis(triphenylphosphine)palladium(0) (724mg, 0.625mmol) in 1 :1 ethanol/toluene (100ml) was stirred and heated at 900C under argon for 3 hours. The mixture was cooled, diluted with water (200ml) and ether (50ml) and the organic phase dried (magnesium sulphate), evaporated and purified by flash chromatography on a Biotage column eluting with 1 :4 ethyl acetate/hexane. The title compound was isolated as a colourless oil (1.8g).LC/MS: Rt=3.19 min, [M+H]+ 306.1 , 308.1 |