Preparation method of 2-substituted-4-(piperidylmethyl) pyridine
A technology of hydroxymethylpyridine and methylmethyl, which is applied in the field of preparation of 2-substituted-4-(piperidinylmethyl)pyridine, can solve the problem of high toxicity to production operators, high requirements for reaction equipment, serious environmental pollution, etc. problems, to achieve the effect of helping environmental protection, less side reactions, and low selection requirements
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[0051] 1. Preparation of N-chlorodiisopropylamine (Chem.Ber.1966,99:1347)
[0052] At 0°C, add 500 milliliters of diisopropylamine dropwise to 1 liter of 6.5% sodium hypochlorite solution. After the dropping is complete, raise the temperature naturally and stir for 1 hour. Separate the organic phase and wash it twice with 1N sulfuric acid. After sodium drying, the desiccant was filtered off to obtain 362 g, yield 75%. 1 H NMR (CDCl 3): δ 1.18 (d, J = 6.0 Hz, 12H), 3.29 (m, 2H).
[0053] 2. Preparation of 2-bromo-4-(piperidinylmethyl)pyridine (Formula 1, R=Br)
[0054] Dissolve 171.3 grams of 2-bromo-4-hydroxymethylpyridine (formula 2, R=Br), 356 grams of triphenylphosphine and 700 milliliters of tetrahydrofuran in a 2L three-necked flask, then add 90.3 milliliters of piperidine, and cool in an ice-water bath to At 10°C, a solution of 133 g of N-chlorodiisopropylamine in 300 ml of tetrahydrofuran was added dropwise, and the mixture was stirred at room temperature for 4 ho...
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