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Chemical Structure| 1035040-11-9 Chemical Structure| 1035040-11-9

Structure of 1035040-11-9

Chemical Structure| 1035040-11-9

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Product Details of [ 1035040-11-9 ]

CAS No. :1035040-11-9
Formula : C27H33ClN4O3
M.W : 497.03
SMILES Code : O=C(NCCN1[C@@H](CN(N=C(CC2=CC=C(Cl)C=C2)C3=C4C=CC=C3)C4=O)CCC1)CCCOC

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Application In Synthesis of [ 1035040-11-9 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 1035040-11-9 ]

[ 1035040-11-9 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 29006-02-8 ]
  • [ 1035042-01-3 ]
  • [ 1035040-11-9 ]
YieldReaction ConditionsOperation in experiment
89% With ammonia; O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate; triethylamine; In methanol; ethanol; N,N-dimethyl-formamide; Preparation (a) 4-(Methyloxy)butanoic acid (for example, as prepared for Intermediate 17) (155 mg, 1.31 mmol) was dissolved in DMF (3 ml) with stirring. Triethylamine (555 mul, 3.98 mmol) was added, followed by TBTU (422 mg, 1.31 mmol) in DMF (2 ml), and the mixture was stirred at room temperature. 2-[(2R)-1-(2-Aminoethyl)-2-pyrrolidinyl]methyl}-4-[(4-chlorophenyl)methyl]-1(2H)-phthalazinone (for example, as prepared for intermediate 19) (401 mg, 1.01 mmol) in DMF (3 ml) was added and the mixture was stirred at room temperature for 2 h. The reaction mixture was applied to a silica cartridge (70 g, pre-conditioned with MeOH) and eluted with MeOH (3 column volumes) then 10% aqueous 0.88 s.g. ammonia in MeOH (3 column volumes). Appropriate fractions were combined and concentrated in vacuo. The residue was redissolved in MeOH and applied to a SCX cartridge (70 g, pre-conditioned with MeOH). The cartridge was washed with MeOH (2 column volumes) and then eluted with 10% 0.880 s.g. ammonia in MeOH (3 column volumes). The appropriate basic fractions were combined and the solvent removed in vacuo. The residue was purified by chromatography on silica (50 g, eluding with DCM-EtOH-aqueous ammonia, 200:8:1 (400 ml), then 150:8:1 (450 ml)). The appropriate fractions were combined and concentrated in vacuo. The sample was redissolved in EtOH and concentrated in vacuo to give the title compound (446 mg, 89%). LCMS RT = 2.86 min, ES+ve m/z 497/499 (M+H)+. 1H NMR (400 MHz, MeOH-d4) delta 8.43-8.36 (m, 1H), 7.96-7.90 (m, 1H), 7.89-7.81 (m, 2H), 7.34-7.27 (m, 4H), 4.36 (s, 2 H), 4.31 (dd, J = 13, 4 Hz, 1H), 4.24 (dd, J = 13, 7 Hz, 1H), 3.41-3.24 (m, 7H), 3.21-3.13 (m, 1H), 3.10-3.00 (m, 2H), 2.55-2.46 (m, 1H), 2.36-2.27 (m, 1H), 2.26 (t, J = 8 Hz, 2H), 1.94-1.68 (m, 6H).
 

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