Analyzing the synthesis route of 115619-01-7

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.115619-01-7,4-(4-Ethylpiperazin-1-yl)phenylamine,as a common compound, the synthetic route is as follows.

[00236] To a 15 mL pressure tube was added 8-ethyl-4-methyl-2-(methylsulfonyl)pyrido[2,3-d]pyrimidin-7(8H)-one (70.0 mg, 0.202 mmol), 1 mL dimethylsulfoxide (dmso), and 4-morpholinoaniline (Aldrich, 72.9 mg, 0.409 mmol, 2 eq,) was added. The reaction mixture was heated to 1000C for 16 h. The reaction was diluted with EtOAc, washed with sat. aqueous NaHCO3, dried over Na2SO4, filtered, and concentrated. The crude material was purified by preparative hplc using 20 – 90% ACN in H2O with 0.05% THF. The desired product containing fractions were combined, diluted with EtOAc, and washed with saturated NaHCO3, H2O, and brine. The organic layer was dried over Na2SO4 and solvent was removed on a rotary evaporator to a colorless film. The film was dissolved in 2 mL ACN and 2 mL H2O, frozen and lyophilized overnight, yielding 8.7 mg (10% yield) of 6-Bromo-8-ethyl-4-methyl-2-[(4-morpholin-4-ylphenyl)amino]pyrido[2,3- EPO phiyrimidin-7(8H)-one as a colorless powder: 1H NMR (400 MHz, CDCl3): delta 8.13 (s, IH),7.56 (d, J= 8.8 Hz5 2H), 7.22 (s, IH)5 6.94 (d, J= 9.2 Hz5 2H), 4.50 (q, J= 7.2 Hz5 2H), 3.88(t, J= 4.4 Hz, 4H)5 3.15 (t, J= 5.2 Hz5 4H)5 1.58 (s, 3H)5 1.35 (t, J= 6.8 Hz, 3H)5 MS (EI) forC20H22BrN5O2: 444.3 (MH+)

115619-01-7, The synthetic route of 115619-01-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; EXELIXIS, INC.; WO2007/44698; (2007); A1;,
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