New downstream synthetic route of 1,3-Dimethoxypropan-2-ol

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,623-69-8, its application will become more common.

Reference of 623-69-8, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 623-69-8 as follows.

To NaH (0.366 g, 9.16 mmol) in THF (12 mL) at 0 ¡ãC was added 1 ,3-dimethoxy-2- propanol (1 g, 8.32 mmol) in THF (8 mL) solution. The mixture was warmed to room temperature and stirred for 0.5 hour. To this was added tosyl chloride (1.587 g, 8.32 mmol) in one portion. The white cloudy mixture was stirred at room temperature for 16 hours. LC/MS showed complete conversion. The reaction mixture was poured into water and extracted with EtOAc. The organic extracts were combined, washed with brine, dried with sodium sulfate and concentrated in vacuo to give 2 g of colorless oil. The crude mixture was purified by column chromatography (silica gel column 80 g, gradient: 0 min, 100percentn-heptane; 5-12 min, 20percent EtOAc in Heptane; 12-15 min. 30percent EtOAc in Heptane and hold until 30 min). The pure fractions were combined and concentrated under reduced pressure to give 1.25 g of product as colorless oil which solidified upon standing

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,623-69-8, its application will become more common.

Reference:
Patent; NOVARTIS AG; ANTONIOS-MCCREA, William R.; BARSANTI, Paul A.; HU, Cheng; JIN, Xianming; LIN, Xiaodong; MARTIN, Eric J.; PAN, Yue; PFISTER, Keith B; RENHOWE, Paul A.; SENDZIK, Martin; SUTTON, James; WAN, Lifeng; WO2012/101065; (2012); A2;,
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