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ChemicalBook CAS DataBase List 2-Picolylamine
3731-51-9

2-Picolylamine synthesis

9synthesis methods
-

Yield:3731-51-9 95.11%

Reaction Conditions:

with 5%-palladium/activated carbon;ammonia;hydrogen in methanol at 30; under 7500.75 Torr; for 8 h;Autoclave;Reagent/catalyst;Temperature;Pressure;

Steps:

9-12 Example 12
One-step synthesis of 2-methylaminopyridine includes the following steps: (1) Add 200 kg of 2-cyanopyridine and 1600 kg of methanol to the pressure reactor, and stir and dissolve, and then add 6 kg of palladium-carbon catalyst with a palladium loading of 5%; (2) After replacing with nitrogen for three times, pass in 40kg ammonia gas under stirring; (3) Pass in hydrogen, and react for 8 hours at a hydrogen pressure of 1.0 MPa and a temperature of 30 ° C; (4) After cooling to room temperature and filtering, the filter residue is recovered as a palladium-carbon catalyst. The filtrate is distilled under reduced pressure at 65 ° C and -0.1 MPa to obtain the product 2-methylaminopyridine, which is a transparent light yellow viscous liquid. Distillation The reaction solvent methanol produced is recovered for use;The yield of the product 2-methylaminopyridine was 95.11%, and its purity by GC (gas chromatography) was 99.94%.

References:

Xi'an Kaili New Materials Co., Ltd.;Zhang Yu;Gao Wu;Xiao Dawei;Yao Qi;Huang Qionglin;Li Xiaoan CN110606827, 2019, A Location in patent:Paragraph 0023-0026

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