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Chemical Structure| 917081-96-0 Chemical Structure| 917081-96-0

Structure of 917081-96-0

Chemical Structure| 917081-96-0

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Product Details of [ 917081-96-0 ]

CAS No. :917081-96-0
Formula : C18H13IN2O3
M.W : 432.21
SMILES Code : O=C1N(C(C2=CC=CC=C2)=O)C(C(C)=CN1C3=CC=C(I)C=C3)=O

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Application In Synthesis of [ 917081-96-0 ]

* 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 [ 917081-96-0 ]

[ 917081-96-0 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 917081-96-0 ]
  • [ 177991-01-4 ]
  • C105H68N8O12 [ No CAS ]
YieldReaction ConditionsOperation in experiment
37% With bis-triphenylphosphine-palladium(II) chloride; copper(l) iodide; triethylamine; In tetrahydrofuran; at 60℃; for 7h;Inert atmosphere; 1,1',1'',1'''-([Methanetetrayltetrakis(benzene-4,1-diyl)]-tetrakis(ethyne-2,1-diyl)}tetrakis(benzene-4,1-diyl))tetrakis[5-methylpyrimidine-2,4(1H,3H)-dione] (19) To a solution of <strong>[177991-01-4]tetrakis(4-ethynylphenyl)methane</strong> (18; 700 mg, 1.68 mmol), 7 (3.47 g, 8.06 mmol), PdCl2(PPh3)2 (58.8 mg, 0.084 mmol), and CuI (32 mg, 0.168 mmol) in anhyd THF (120 mL) was added Et3N (9.3 mL, 67.20 mmol) at RT. The reaction mixture was stirred at 60 C for 7 h under N2. The mixture was directly evaporated and the residue was subjected to column chromatography (CH2Cl2/EtOAc 10:1) to afford the protected thymine tetramer as a white solid (1.02 g, 37%).The protected thymine tetramer (1.02 g, 0.63 mmol) from above was dissolved in MeOH (30 mL) and hydrazine hydrate (1.2 mL, 25.0 mmol) was added. The mixture was stirred at 100 C for 9 h. The mixture was cooled to RT and filtered. The precipitate was dried in vacuo; yield: 682 mg (33% over 2 steps); white powder; mp: 263-265 C. 1H NMR (300 MHz, DMSO-d6): = 11.36 (br, 1 H), 7.66 (s, 1 H), 7.64 (s, 2 H), 7.60-7.57 (d, J = 8.4 Hz, 1 H), 7.50-7.47 (d, J = 8.4 Hz, 2 H), 7.24- 7.22 (d, J = 8.4 Hz, 2 H), 1.81 (s, 3 H). 13C NMR (125 MHz, DMSO-d6): = 164.1, 150.0, 145.8, 140.7, 138.9, 131.9, 131.1, 130.6, 127.0, 121.6, 120.1, 109.5, 89.6, 88.8, 64.3, 11.7.HR-MALDI: m/z [M + H]+ calcd for C77H53N8O8: 1217.3981; found: 1217.3971.
 

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