Related Products of 930-36-9,Some common heterocyclic compound, 930-36-9, name is 1-Methylpyrazole, molecular formula is C4H6N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Methylpyrazole (4.1 g, 50 mmol, 1 equiv) and anhydrous DMF (11.6 ml, 3 equiv) were placed in a 100 ml of two-neck flask which was equipped with a Allihn condenser (a CaC12 drying tube was connected thereto) and a constant- pressure dropping thnnel, and the flask was placed in the oil bath of 90 C. Phosphorus oxychloride (5.6 ml, 1.2 equiv) was added dropwise over a period of 1 h. After the addition was completed, the mixture was stirred for a further 2 h. Then the solution was cooled and poured into a lot of ice water. The resulting mixture was brought to pH 4-5 with a solution of 10% NaOH solution and then extracted with dichloromethane several times until the product in the aqueous phase is little. The combined organic phase was washed with a small amount of brine twice, dried over MgSO4, filtered and then evaporated in vacuo to give the crude product of 1-me- thyl-1H-pyrazole-4-carbaldehyde, which can be directly used in the next step without further separation.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Methylpyrazole, its application will become more common.
Reference:
Patent; Shen, Jianhua; Wang, Yiping; Wang, Kai; US2014/171431; (2014); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics