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Chemical Structure| 264264-31-5 Chemical Structure| 264264-31-5

Structure of 264264-31-5

Chemical Structure| 264264-31-5

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Product Details of [ 264264-31-5 ]

CAS No. :264264-31-5
Formula : C17H23NO3
M.W : 289.37
SMILES Code : O=C(N1CCC2=CC=C(C(C)=O)C=C2CC1)OC(C)(C)C
MDL No. :MFCD12408164

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Application In Synthesis of [ 264264-31-5 ]

* 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 [ 264264-31-5 ]

[ 264264-31-5 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 264264-31-5 ]
  • [ 27258-32-8 ]
  • [ 1204828-81-8 ]
YieldReaction ConditionsOperation in experiment
With 1,8-diazabicyclo[5.4.0]undec-7-ene; lithium chloride; In acetonitrile; for 1h;Molecular sieve; /.7.1 Intermediate 21; A 25ml round-bottomed flask was charged with lithium chloride (0.366 g, 8.64 mmol), 1 -methyl- lH-pyrazole- 3-carbaldehyde (0.951 g, 8.64 mmol), and tert-butyl 7-acetyl-4,5-dihydro-lH-benzo[d]azepine-3(2H)- carboxylate (2.5 g, 8.64 mmol) in acetonitrile (10 ml) to give a colourless solution. DBU (1.302 ml, 8.64 mmol) was added and 4A molecular sieves. The reaction was stirred for one hour.The solvent was evaporated and the residue was taken up into ethyl acetate and washed with 5percent citric acid (x2), saturated sodium bicarbonate, and dried and evaporated. The residue was purified by Biotage 5Og SNAP column using 50percent EtOAc/ Petrol to yield pure (E)-tert-butyl 7-(3-(l-methyl-lH-pyrazol-3-yl)acryloyl)-4,5-dihydro-lH- benzo[d]azepine-3(2H)-carboxylate (6.82 mmol)MS ES+ : 3261H NMR (400 MHz, MeOD): delta 7.80 - 7.85 (m, 2H), 7.64 - 7.66 (m, 2H), 7.60 - 7.63 (m, IH), 7.27 - 7.32 (m, IH), 6.75 - 6.78 (m, IH), 3.92 (s, 3H), 3.56 (br. s., 4H), 2.95 - 3.02 (m, 4H), 1.44 (s, 9H)
 

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