Reference of 890094-38-9, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 890094-38-9, name is 2-Chloro-N-isopropyl-5-nitropyrimidin-4-amine. A new synthetic method of this compound is introduced below.
Step 2(3a) (4a)Compound (3a) (90.9 g, 0.420 mol), tetrahydrofuran (840 mL, abs.), Pt/C 5% (9.0 g, 42 mmol) and vanadyl acetylacetonate (4.5 g, 16 mmol) are added in a Parr apparatus and shaken under a hydrogen pressure of 50 psi at 20 C to 40 C for several hours until the reduction of the nitro group is complete (TLC control: silica gel, CH : EE = 1 : 1 ). The catalyst is removed and the solvent is evaporated under reduced pressure. The crude product is dissolved in a mixture of tetrahydrofuran (100 mL) and isopropanol (120 mL) and transferred into a three necked flask. Trimethylchlorosilane (54 ml) is added dropwise and the hydrochlorid precipitates. The suspension is stirred for 16 hours. The precipitate is suction filtered and dried. Yield: 54.8 g (59 % of theory) of compound (4a) as brown crystalline solid.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,890094-38-9, 2-Chloro-N-isopropyl-5-nitropyrimidin-4-amine, and friends who are interested can also refer to it.
Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; LINZ, Guenter; BISCHOFF, Daniel; EBNER, Thomas; WO2011/101369; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia