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ChemicalBook CAS DataBase List tert-butyl 4-nitropiperidine-1-carboxylate
1228630-89-4

tert-butyl 4-nitropiperidine-1-carboxylate synthesis

4synthesis methods
301673-14-3 Synthesis
N-Boc-4-iodopiperidine

301673-14-3
210 suppliers
$10.00/1g

-

Yield:1228630-89-4 290 g

Reaction Conditions:

with 3,5-dihydroxyphenol;sodium nitrite in dimethyl sulfoxide at 45;Inert atmosphere;

Steps:

2
Raw material 2 (1000 g, 2.67 mol), sodium nitrite (368 g, 5.33 mol) and phloroglucinol (538 g, 4.27 mol) were dissolved in DMS0 (4 L) in a reaction flask and then under nitrogen Stir at 45 ° C overnight. Products in petroleum ether:Ethyl acetate (volume ratio) = 5: 1, the rf value was about 0.3. After completion of the reaction, 20 L of water was added and stirred for 30 minutes. Then, the mixture was extracted with a mixed solvent of petroleum ether: ethyl acetate (v / v) = 5: 1, and whether or not the extraction was complete (with ninhydrin). The organic phase was washed with saturated NaCl, dried over sodium sulfate and concentrated to give the crude product. The crude product was purified by column chromatography to give 290 g of an oil product.

References:

wuxi apptec (shanghai) co. ltd;Zhang, Xuhua;Guo, Aixin;Ma, Jianyi;Jiang, Luyong;Ma, Rujian CN103130708, 2016, B Location in patent:Paragraph 0019; 0021

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