ChemicalBook CAS DataBase List 2-Chloro-N-methylnicotinamide

2-Chloro-N-methylnicotinamide synthesis

5synthesis methods

Product Name:2-Chloro-N-methylnicotinamide
CAS Number:52943-20-1
Molecular formula:C7H7ClN2O
Molecular Weight:170.6

20604-88-0
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52943-20-1
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Yield:52943-20-1 98.36 %

Reaction Conditions:

with triethylamine hydrochloride in 1,2-dichloro-ethane at 65;

Steps:

2 Example 2 N-methyl-2-chloronicotinamide

The catalyst supports 8% tin chloride, 1% zinc, and the balance is silica powder. Add the above raw materials in an appropriate amount of methanol solvent according to the formula ratio, stir at about 30°C for 48h, slowly increase the temperature, evaporate the solvent methanol to dryness, and activate at 450°C to obtain solid catalyst;Weigh 47.4g (0.5mol) of 3-chloroacrolein with a purity of 95%, 58g (0.58mol) of 2-cyano-N-methyl-acetamide with a purity of 98%, and 189.5g of dichloroethane in a reaction flask Dissolve, add 8.3g of triethylamine hydrochloride, raise the temperature to 65°C, and take a sample after 4 hours of heat preservation reaction to detect 0.12% of 3-chloroacrolein by HPLC, and end the reaction; cool down to 40°C and add 8g of composite catalyst, at this temperature Stir for 2 hours, gradually increase the temperature and keep warm, keep warm for 0.5h every time the temperature rises by 10°C, keep warm for 0.5h at 80°C, take a sample to detect 0.08% of intermediate I remaining in the ultra-high performance liquid phase, and the heat preservation is over; filter and recover the catalyst while it is hot, add 0.5g of activated carbon to the Decolorize at about 50°C for 0.5h, filter, evaporate the solvent to dryness, and quickly cool and slice to obtain 86g of the target product of N-methyl-2-chloronicotinamide, with a content of 97.5% and a yield of 98.36%.

References:

CN115260092,2022,A Location in patent:Paragraph 0038-0041

2942-59-8 Synthesis