With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.768-66-1,2,2,6,6-Tetramethylpiperidine,as a common compound, the synthetic route is as follows.
EXAMPLE 1 Preparation of (2,2,6,6-tetramethyl-piperidine) N-oxide (TEMPO) An organic solution consisting of 5 g of 2,2,6,6-tetramethylpiperidine (i.e. 0.0354 mol) dissolved in 20 ml of dichloromethane is prepared with stirring in a 100 ml round-bottomed flask fitted with 2 dropping funnels, a condenser, a pH-measuring probe and a stirrer. 20 ml of water are then added to this solution so as to have a two-phase system. Next, 10.8 g of a 40% solution of peracetic acid 4n acetic acid and aqueous 35% by weight K2CO3 solution are introduced (with stirring) slowly and simultaneously. The molar amount of peracetic acid introduced is 0.0568 mol, which corresponds to a peracetic acid/amine molar ratio of 1.6. The amount of aqueous K2CO3 solution is adjusted such that the pH of the aqueous phase of the two-phase medium is maintained at between 7.2 and 7.5 in the course of the addition. 20 minutes after the addition, the total disappearance of the amine and the formation of TEMPO are found by gas chromatography (GC). The reaction is stopped and K2CO3 solution is added so as to obtain a pH equal to 9, and the red-colored TEMPO is then extracted with CH2Cl2. Evaporation of the solvent gives 4.9 g of TEMPO with a melting point equal to 36 C. The purity of the TEMPO is checked by GC relative to a sample of pure product (purity greater than 99%) sold by the company Aldrich. Mass spectrum (m/e): 157 (M+1), 768-66-1
The synthetic route of 768-66-1 has been constantly updated, and we look forward to future research findings.
Reference：
Patent; Atofina; US6538141; (2003); B1;,
Piperidine – Wikipedia
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