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Chemical Structure| 799796-66-0 Chemical Structure| 799796-66-0

Structure of 799796-66-0

Chemical Structure| 799796-66-0

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Product Details of [ 799796-66-0 ]

CAS No. :799796-66-0
Formula : C11H14N2O
M.W : 190.24
SMILES Code : O=C1N(C)CCNC1C2=CC=CC=C2
MDL No. :N/A

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Application In Synthesis of [ 799796-66-0 ]

* 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 [ 799796-66-0 ]

[ 799796-66-0 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 799796-66-0 ]
  • [ 5271-27-2 ]
YieldReaction ConditionsOperation in experiment
Lithium aluminium hydride (3.04 g, 0.8 moles) was suspended in tetrahydrofuran (60 ml) under nitrogen atmosphere. A solution of 1-methyl-2-oxo-3-phenylpiperazine (10 g in 10 ml of tetrahydrofuran) was added at 10-15° C. Slowly, raised the temperature of reaction mass and refluxed for 2 hours. Cooled the reaction mass to 5° C. and quenched successively with 3 ml of water, 3 ml of 15percent aqueous sodium hydroxide solution and 9 ml of water. Reaction mass was stirred for 1 hour at 25-30° C. Filtered the reaction mass and the filtrate was concentrated under reduced pressure. Dissolved the residue in DM water (25 ml) and concentrated hydrochloric acid (8 ml) and the solution was washed with cyclohexane (20 ml). pH was adjusted to 11.0-12.0 with 50percent w/w aqueous sodium hydroxide solution and extracted the product with methylene chloride (2.x.50 ml). Methylene chloride layer was concentrated under reduced pressure and 7.54 g of pure 1-Methyl-3-phenylpiperazine was isolated in cyclohexane having HPLC purity 99.7percent. [0034] 1H NMR (300 MHz) in CDCl3: delta(ppm); 1.80 (bs, 1H), 1.95-2.18 (m, 2H), 2.31 (s, 3H), 2.79-3.12 (m, 4H), 3.85-3.89 (m, 1H), 7.23-7.40 (m, 5H).
 

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