139009-66-8, (S)-N-Boc-2,2-dimethyloxazolidine-4-carboxylic Acid is a oxazolidine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
Before being used, the reactor was freed with DCM, dried under vacuum and purged by flushing with nitrogen for 15 to 30 min, the Erlenmeyer flask is rinsed with amylene-stabilized DCM and then dried under nitrogen. The reactor was charged with 95 ml of DCM and 34.0 g of boc-L-serine acetonide, cooled to 4-10 C. and 14.3 g of N-methylmorpholine were added using a dropping funnel while maintaining the temperature at 4-10 C. The dropping funnel was rinsed with 2.5 ml of DCM. 17.1 g of pivaloyl chloride were added using a dropping funnel while maintaining the temperature at 4-10 C. and the dropping funnel was rinsed with 2.5 ml of DCM. The mixture is kept stirred at 4-10 C. for 2 h.A solution of aminobal (20.0 g) in DCM (95 ml) was prepared with stirring and this solution was added to the reactor while maintaining the temperature at 4-10 C. The mixture was subsequently heated to 20 C. over 1 h and was kept stirred at 20 C. for a minimum of 16 h. 100 ml of demineralized water was added to the reactor at 20-25 C. and the mixture was left stirring for 20 min and separated by settling. The lower organic phase comprising the product and the upper phase (predominantly aqueous) were withdrawn. The organic phase comprising the product was again charged to the reactor. 140 ml of a 1.0 N aqueous sodium hydroxide solution were added. The mixture was kept stirred at 20-25 C. for approximately 20 min and then allowed to separate by settling. The lower organic phase comprising the product was withdrawn. The organic phase comprising the product was again charged to the reactor. 100 ml of demineralized water were added. The mixture was kept stirred at 20-25 C. for approximately 20 min and then allowed to separate by settling. The lower organic phase comprising the product was withdrawn. The organic phase comprising the product was again charged to the reactor. 100 ml of isopropanol was added.Distillation was carried out (35+/-5 C. in the jacket) under a residual pressure of approximately 30 mbar until a residual volume of 100 ml was present in the reactor. The temperature was adjusted to 20 C. and the mixture was left stirring at 20 C. for 3 h. The reactor was rinsed and the cake was washed twice with a total volume of 40 ml of isopropanol. The product was dried at 40 C. under a vacuum of 30 mbar. Yield of isolated product: 60%., 139009-66-8
139009-66-8 (S)-N-Boc-2,2-dimethyloxazolidine-4-carboxylic Acid 6932187, aoxazolidine compound, is more and more widely used in various fields.
Reference£º
Patent; C/O SANOFI; US2012/302759; (2012); A1;,
Oxazolidine – Wikipedia
Oxazolidine | C3H7NO – PubChem