Extracurricular laboratory: Synthetic route of 2,4-Dichloropyrimidine-5-carbonitrile

The synthetic route of 3177-24-0 has been constantly updated, and we look forward to future research findings.

Related Products of 3177-24-0 , The common heterocyclic compound, 3177-24-0, name is 2,4-Dichloropyrimidine-5-carbonitrile, molecular formula is C5HCl2N3, its 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.

2,4-Dichloropyrimidin-5-carbonitrile (1.00 g, 5.75 mmol) was dissolved in 30 mL DMF. To it were added (R)-2-aminobutanamide hydrochloride (1.20 g, 8.62 mmol) and DIEA (3.0 mL, 17.24 mmol). The mixture was stirred at 50°C for 10 m to afford two coupling product in about equal amount in quantitative yield. The mixture was concentrated in vacuo, diluted with EtOAc, washed with brine twice, dried, concentrated and subjected to flash column to separate (R)-2-((4-chloro-5-cyanopyrimidin-2-yl)amino)butanamide.The mixture of (R)-2-((4-chloro-5-cyanopyrimidin-2-yl)amino)butanamide (400 mg, 1.7 mmol), 3-methylisothiazol-5-amine hydrochloride (770 mg, 5.1 mmol), fine powder Cs2C03 (3.88 g, 11.9 mmol), BINAP (212 mg, 0.34 mmol) and Pd(OAc)2 (77 mg, 0.34 mmol) in 50 mL dioxane was degassed using argon stream and stirred at 105°C under argon atmosphere for 6 h. It was diluted with 400 mL EtOAc, vigorously stirred, filtered through celite, concentrated in vacuo and subjected to flash column to isolate (R)-2-((4-chloro-5-cyanopyrimidin-2- yl)amino)butanamide (210 mg).

The synthetic route of 3177-24-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PORTOLA PHARMACEUTICALS, INC.; JIA, Zhaozhong J.; KANE, Brian; XU, Qing; BAUER, Shawn M.; SONG, Yonghong; PANDEY, Anjali; DICK, Ryan; WO2013/78468; (2013); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia