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ChemicalBook CAS DataBase List tert-butyl 2-oxo-8-azaspiro[4.5]decane-8-carboxylate

tert-butyl 2-oxo-8-azaspiro[4.5]decane-8-carboxylate synthesis

3synthesis methods
-

Yield: 72%

Reaction Conditions:

with potassium hydroxide in tetrahydrofuran;methanol;water at 0 - 20; for 24 h;Temperature;Solvent;

Steps:

3
A solution of 10% to 40% aqueous potassium hydroxide (20 mL) was added to a solution of tert-butyl-2-carbonyl-7-spiro [3.5] nonane-7-carboxylic acid (8.2 g) in tetrahydrofuran and methanol Ratio: 10/1 to 1/10) in a mixed solvent,N-methyl-N-nitro-p-toluenesulfonamide (19.6 g) was dissolved in 300 ml of water,And the mixture was added dropwise to the above reaction solution at 0 ° C, followed by reaction at room temperature for 24 hours. Raw material reaction is complete, the system cooled to room temperature, add acetic acid quenching spin dry,Then dissolved in ethyl acetate (100 mL)Washed with water (100 mL) and saturated brine (100 mL), respectively.Then dried over anhydrous sodium sulfate, filtered, dried under reduced pressure,Tert-butyl-2-carbonyl-8-spiro [4.5] decane-8-carboxylic acid (6.6 g, yield: 72%) was obtained by column chromatography.

References:

CHANGZHOU HEQUAN PHARMACEUTICAL CO LTD;Shanghai Syn-The-All medical research and development Co . ltd;Qian, guolei;Mao, yanjun;Chen, Linlin;Zhou, jiang;Li, Hong;Tang, xiaowu;Yang, caimin;Zhang, TongXin;Sun, Wei;Yu, Leng Bo;He, zhenmin;Ma, RuJian;Chen, minzhang;Fu, XiaoYong;Wang, WenGui CN105272914, 2016, A Location in patent:Paragraph 0010; 0014

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