A kind of preparation method of pharmaceutical intermediate n-boc-3-piperidone
A N-BOC-3-, intermediate technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of expensive oxidants, environmental pollution, high manufacturing costs, and achieve catalytic properties. The effect of maintaining stability, avoiding environmental pollution and reducing production costs
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preparation Embodiment 1
[0046]Set up the reaction device, add 215g of disodium hydrogen phosphate dodecahydrate and 600ml of water into the reaction bottle, stir to dissolve, cool down to below 10°C with ice water, add 35.3g of ammonium chloride, 109.6g of acetone dicarboxylate acid, stirring to dissolve until clear. At 5°C, add 120.1g of glutaraldehyde and 120g of water to the reaction flask, stir to make the reaction complete, and the pH of the reaction solution is measured to be 4.5; remove the ice bath, and warm up to room temperature with 35°C of warm water. After stirring overnight, gas evolved. The next morning, the reaction solution was seen to be light yellow, basically no gas was emitted, and the measured pH of the reaction solution was 6.0; the pH of the reaction solution was adjusted to 8.5-9.5 with 40% NaOH, and about 30 g of NaOH was used; after adding NaOH, Add 250ml of methanol, stir evenly, and cool down with an ice-water bath; then add 144g of di-tert-butyl dicarbonate to the react...
preparation Embodiment 2
[0048] Set up the reaction device, add 23.9g of 3-oxo-9-azabicyclo[3,3,1]nonane-9-carboxylate tert-butyl ester and 239ml of methanol into a 500ml three-neck flask, and stir until the reaction The liquid was clear and transparent, and was cooled to 0°C with an ice-salt bath, and 4.5 g of NaBH was slowly added to the reaction liquid in batches. 4 , a small amount of gas is released during the addition process; NaBH 4 After the addition was complete, it was stirred in an ice-salt bath until the reaction was complete; the reaction solution was clear and transparent at 10°C. Pour the reaction solution into 400ml of ice water made from 12ml of concentrated hydrochloric acid, stir evenly, extract three times with 400ml of dichloromethane × 3, combine the organic phase and wash with 300ml of water, concentrate the organic phase under reduced pressure, and obtain a light yellow viscous liquid after concentration 25g, the yield of the crude product is about 100%, the obtained liquid so...
preparation Embodiment 3
[0050] Set up the device, add 240ml of anhydrous DMF and 24.0g of cross-linked polystyrene chloride balls to a 500ml three-necked bottle, stir at room temperature under nitrogen protection to make it fully swell; Moderate swelling; after swelling, the reaction solution is light yellow and turbid, add 24.1g of tert-butyl 3-hydroxy-9-azabicyclo[3,3,1]nonane-9-carboxylate to it and stir evenly, and the solution becomes bright yellow ; Add 5g of sodium hydrogen to the solution, make the solution stir and react at this temperature (35°C) for 30min; put the reaction bottle into an oil bath at 60°C, make it react completely, the solution is yellow and turbid, stop heating, and cool down naturally And stir overnight; at 32°C, the appearance of the reaction solution has no obvious change, add 200ml of water to it, stir evenly, filter under reduced pressure, wash the filter cake with 500ml×2 water, and drain as much as possible to obtain a khaki solid cross-linked Polystyrene microspher...
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