Electric Literature of 1100318-96-4, Adding some certain compound to certain chemical reactions, such as: 1100318-96-4, name is 4-Iodo-7H-pyrrolo[2,3-d]pyrimidine,molecular formula is C6H4IN3, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 1100318-96-4.
[00349] 4-lodopyrrolo[2,3-d]pyrimidine(2b, 50.3 g, 95.5% purity, 196 mmol) was dissolved/suspended in 0.64 L of anhydrous THF in a three- necked 2 L round bottom flask under nitrogen atmosphere, equipped with a mechanical stirrer and a thermometer. The solution was cooled down to -15 0C in a dry ice-acetone bath and 206 ml_ of a 1.0 M o-tolylmagnesium chloride THF solution (1.05 equiv.) was added slowly, so the internal temperature would not exceed -10 C. During the addition all of the solids dissolved. The cooling bath was removed and 104 ml_ of a 1.95 M isopropylmagnesium chloride THF solution (1.03 equiv.) was added over a period of 3 minutes. During the addition tan solids precipitate; the stirring should be vigorous to avoid clumping. The resulting solution was warmed rapidly to room temperature using warm water bath. To this suspension, 59.9 g of the nitrile sodium salt (19, 0.77 equiv.) in 120 ml_ dry THF was added and the resulting mixture was stirred at 45 C for 16 hours. The mixture was cooled down in an ice bath and 101 mL of 36% aqueous HCI was added dropwise, so the internal temperature would not exceed 30 C, while vigorously stirred. Yellow solids precipitated and the entire thick suspension was mechanically stirred for 30 minutes at 50 0C (yellow solids become orange), cooled down to room temperature and then filtered. The solids were washed with 700 mL of THF, followed by 700 mL of diethyl ether, followed by two 1 L portions of 1 M aqueous HCI. The resulting wet orange solid was taken up in a mixture of 0.9 L ethyl acetate, 0.5 L water and 50 g of sodium bicarbonate and stirred until completely dissolved. The solution was filtered through a pad of CELITE and the layers were separated. The aqueous layer was extracted with 50 mL of ethyl acetate. The combined organic layers were filtered through a pad of
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 1100318-96-4, 4-Iodo-7H-pyrrolo[2,3-d]pyrimidine, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; CHEMOCENTRYX, INC.; WO2009/9740; (2009); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia