768-66-1, 2,2,6,6-Tetramethylpiperidine is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
768-66-1, 2,2,6,6-Tetramethylpiperidine (2.78 g) was dissolved in anhydrous chloroform (80 ml), and triethylamine (10.1 g) was added thereto. Subsequently, chloroglyoxylic acid ethyl ester (5.40 g) dissolved in anhydrous chloroform (5 ml) was added at 0C, and the mixture was stirred at room temperature for 20 hr. A saturated aqueous sodium hydrogencarbonate solution was added thereto, and the organic layer was separated. The organic layer was washed with saturated brine and was dried over anhydrous sodium sulfate, and the solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography on silica gel, eluting with n-hexane : ethyl acetate (4 : 1) mixed solvent to give N-(glyoxylic ethyl ester)-2,2,6,6-tetramethylpiperidine (4.50 g, yield 94%). 1H-NMR (CDCl3, 400 MHz): 0.85 (t, J = 6.8 Hz, 3H), 1.46 (s, 12H), 1.67 (s, 3H), 4.25 (q, J = 6.8 Hz, 2H) N-(Glyoxylic ethyl ester)-2,2,6,6-tetramethylpiperidine (4.50 g) was dissolved in tetrahydrofuran (100 ml), lithium aluminium hydride (2.14 g) was added thereto at 0C, and the mixture was then heated under reflux for one hr. The excess reagent was decomposed with sodium sulfate decahydrate, followed by filtration through Celite. The filtrate was concentrated under the reduced pressure to give the title compound (3.40 g, yield 100%). 1H-NMR (CDCl3, 400 MHz): 1.02 (s, 12H), 1.41 – 1.65 (m, 6H), 2.68 – 2.72 (m, 2H), 2.95 (br s, 1 H), 3.41 – 3.45 (m, 2H)
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Reference：
Patent; KIRIN BEER KABUSHIKI KAISHA; EP1566379; (2005); A1;,
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