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ChemicalBook CAS DataBase List 1-Boc-3-hydroxypiperidine
85275-45-2

1-Boc-3-hydroxypiperidine synthesis

8synthesis methods
6859-99-0 Synthesis
3-Hydroxypiperidine

6859-99-0
416 suppliers
$6.00/5g

24424-99-5 Synthesis
Di-tert-butyl dicarbonate

24424-99-5
833 suppliers
$13.50/25G

-

Yield:85275-45-2 99%

Reaction Conditions:

with triethylamine in methanol at 20; for 15 h;

Steps:

34.1 1)
1) 3-Hydroxypiperidine-1-carboxylic acid tert-butyl ester Triethylamine (15.2 mL) and a solution of di-tert-butoxydicarbonate (11.9 g) in methanol (50 mL) were added to a solution of 3-hydroxypiperidine (5.00 g) in methanol (50 mL) at room temperature, and the mixture was stirred for 15 hours. The solvent of the reaction mixture was evaporated under reduced pressure, and the residue was purified through silica gel column chromatography (ethyl acetate - chloroform), to thereby give 3-hydroxypiperidine-1-carboxylic acid tert-butyl ester as a solid product (9.86 g, 99%). 1H-NMR(400MHz,CDCl3)δ:1.36-1.55(2H,m), 1.45(9H,s), 1.71-1.78(1H,m), 1.88(1H,m), 3.02-3.13(2H,m), 3.52(1H,m), 3.72-3.76(2H,m). EI-MS m/z:201 (M+).

References:

DAIICHI PHARMACEUTICAL CO., LTD. EP1762568, 2007, A1 Location in patent:Page/Page column 49-50

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