As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 934524-10-4, name is 2,4-Dichloro-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine, molecular formula is C13H9Cl2N3O2S, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. COA of Formula: C13H9Cl2N3O2S
Example 116; 2-[(2-{[1-(lambda/,lambda/-dimethylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-1H-pyrrolo[2,3-c/]pyrimidin-4-yl)amino]-6-fluoro-lambda/-methylbenzamide; Step A/Intermediate D4: 2-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7/-/-pyrrolo[2,3- c/]pyrimidin-4-yl}amino)-6-fluorobenzoic acid; A slurry of 2,4-dichloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidine (50 g, 146 mmol) and 2-amino-6-fluorobenzoic acid (27.2 g, 175 mmol) (for instance from Acros Organics, Belgium) in iPrOH (1200 ml.) and 30 ml. of DIEA was heated to reflux. After 1 h, the solution turned a clear brown color, at which time about 450 ml_ of solvent were removed via distillation. The remaining mixture was treated with DIEA (90 ml.) and heated to reflux for 16 hours. The reaction mixture was then further concentrated by distilling more solvent off (400 ml. over 4 hours), then continued heating at reflux overnight. The resulting mixture was cooled to room temperature and concentrated under reduced pressure to obtain a thick oil which was diluted with EtOAc (1.3 L), then sequentially washed with a 1 N HCI solution (2×500 ml_), and a saturated NaHCOs solution (500 ml_). Further dilution of the separated organic layer with a saturated NaCI solution (500 ml.) led to the formation of a thick precipitate. The entire mixture was filtered and the solid was washed with Et2O. The solid was dried overnight in a vacuum oven at 60 0C to obtain 2-({2-chloro-7-[(4- methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluorobenzoic acid as a yellow solid (61.63 g, 92%). 1H NMR (400 MHz, DMSO-d6) delta ppm 2.37 (s, 3 H), 6.67 (d, J=3.85 Hz, 1 H), 6.71 – 6.81 (m, 1 H), 7.31 (td, J=8.33, 6.04 Hz, 1 H), 7.48
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Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2009/20990; (2009); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia