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ChemicalBook CAS DataBase List N-TERT-BUTOXYCARBONYL-4-(4-TOLUENESULFONYLOXYMETHYL)PIPERIDINE
166815-96-9

N-TERT-BUTOXYCARBONYL-4-(4-TOLUENESULFONYLOXYMETHYL)PIPERIDINE synthesis

8synthesis methods
-

Yield: 85%

Reaction Conditions:

in diethyl ether;tert-butyl methyl ether

Steps:

9.c Preparation of Compound 9 in Table 2
c) 1,4-Diazabicyclo[2.2.2]octane (42.4 g, 0.378 mol) was added to a solution of 4-hydroxymethyl-1-tert-butyloxycarbonylpiperidine (52.5 g, 0.244 mol) in tert-butyl methyl ether (525 ml) and the reaction stirred at ambient temperature for 15 minutes. The reaction was cooled to 5° C. and a solution of 4-toluenesulphonyl chloride (62.8 g, 0.33 mmol) in tert-butyl methyl ether (525 ml) was added dropwise over 2 hours while maintaining the temperature at 0° C. The reaction was stirred at ambient temperature for 1 hour, isohexane was added and the resultant precipitate was collected by suction filtration. Solvent evaporation in vacuo afforded a solid which was dissolved in diethyl ether (250 ml) and washed successively with 0.5N aqueous hydrochloric acid (2*500 ml), water, saturated sodium hydrogen carbonate and brine. Solvent evaporation and drying in vacuo yielded 4-(4-methylphenylsulphonyloxy-methyl)-1-tert-butyloxy-carbonylpiperidine (76.7 g, 85% yield) as a white solid: 1H NMR (CDCl3): 7.80 (d, 2H), 7.35 (d, 2H), 4.00-4.20 (s, 2H), 3.85 (d, 1H), 2.55-2.75 (m, 2H), 2.45 (s, 3H), 1.75-1.90 (m, 2H), 1.65 (d, 2H), 1.45 (s, 9H), 1.00-1.20 (m, 2H): MS (+ve ESI): 392 (M+Na)+.

References:

AstraZeneca AB US7235559, 2007, B1

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