3-PYRIDINECARBOXAMIDE, 4-(2-METHYLPHENYL)-6-(4-METHYL-1-PIPERAZINYL)- synthesis
- Product Name:3-PYRIDINECARBOXAMIDE, 4-(2-METHYLPHENYL)-6-(4-METHYL-1-PIPERAZINYL)-
- CAS Number:342417-01-0
- Molecular formula:C18H22N4O
- Molecular Weight:310.39
109-01-3
342417-00-9
342417-01-0
Step 3: 1.0 g (4.05 mmol) of 6-chloro-4-o-tolylnicotinamide was dissolved in 9.0 mL of N-methylpiperazine, heated to 100 °C and the reaction was maintained for 2 hours. Upon completion of the reaction, the excess N-methylpiperazine was removed by high vacuum distillation. The residue was purified by silica gel column chromatography using dichloromethane as eluent to give 1.2 g (95% yield) of the target compound, 6-(4-methylpiperazin-1-yl)-4-(o-tolyl)nicotinamide, the product was a pale yellow crystalline foam. Mass spectrometry (ISP): m/z 311 ([M+H]+, 100%), 254 (62%).
881743-64-2
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Yield:342417-01-0 88%
Reaction Conditions:
with methanesulfonic acid at 400; for 5 h;
Steps:
1 Synthesis of intermediate A-4
Intermediate A-3 (582 mg, 1.625 mg) was dissolved in 10 ml of methanesulfonic acid and warmed to 100 ° C for 5 h. The reaction solution was poured into ice water and extracted with methyl tert-butyl ether.After the organic phase was combined, it was washed twice with water, the aqueous layer was combined, and the pH was adjusted to 14 with NaOH, and then extracted with methyl tert-butyl ether. The second organic layer was combined, washed successively with water, saturated brine, anhydrousDry over sodium sulfate.Pressurized distillation,The intermediate A-4 was purified to give a yield of 88%.
References:
Beijing Kuanhou Pharmaceutical Technology Co., Ltd.;Cui Yimin;He Long;Ouyang Liang;Gou Maling;Wang Ling CN109384712, 2019, A Location in patent:Paragraph 0107; 0109; 0118; 0119
109-01-3
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