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Chemical Structure| 880160-69-0 Chemical Structure| 880160-69-0

Structure of 880160-69-0

Chemical Structure| 880160-69-0

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Product Details of [ 880160-69-0 ]

CAS No. :880160-69-0
Formula : C21H20FN3O3
M.W : 381.40
SMILES Code : O=C(OC)N(CC1=CC=C(C(N2)=C(C3=C2C=C(F)C=C34)CCNC4=O)C=C1)C

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Application In Synthesis of [ 880160-69-0 ]

* 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.

  • Upstream synthesis route of [ 880160-69-0 ]

[ 880160-69-0 ] Synthesis Path-Upstream   1~1

  • 1
  • [ 880160-69-0 ]
  • [ 283173-50-2 ]
YieldReaction ConditionsOperation in experiment
88%
Stage #1: at 20℃; for 46 h;
Stage #2: With sodium hydroxide In water at 0 - 35℃;
Example 13
Synthesis of 8-Fluoro-2-(4-methylaminomethyl-phenyl)-1,3,4,5-tetrahydro-azepino[5,4,3-cd]indol-6-one (15)
Lactam 14 (14.42 g, 0.038 mol) was dissolved in hydrobromic acid in acetic acid (30percent-32percent, 140 ml).
The reaction solution was stirred for 46 hours at room temperature in a 500 ml flask that was connected to an ethanolamine scrubber system. HPLC analysis indicated the completion of the reaction.
Ice (30 g) was added to the reaction solution followed by addition of aqueous NaOH (327 ml, 10 M, 3.27 mol) while the temperature was maintained between 25° C. and 35° C.
When addition of NaOH was complete, the pH was 10.
The resulting solid was collected by filtration, washed with water (2*50 ml).
The filter cake was then suspended in water (125 ml) and stirred for 2 hours.
The solid was collected by filtration, washed with water (2*25 ml) and dried to afford 10.76 g of product (88percent yield).
1H NMR (300 MHz, DMSO-d6) δ 2.577(s, 3H), 3.053(m, 2H), 3.406(m, 2H), 4.159(s, 2H), 7.36(dd, 1H, J=2.4 Hz and J=9.3 Hz), 7.44(dd, 1H, J=2.4 Hz and J=11.1 Hz), 7.63(d, 2H, J=8.1 Hz), 7.70(d, 2H, J=8.1 Hz), 8.265(t, 1H, J=5.7 Hz), 11.77(s, 1H).
Exact mass calculated for C19H19FN3O: 324.1512. Found: 324.1497.
References: [1] Patent: US2006/63926, 2006, A1, . Location in patent: Page/Page column 6; 11.
 

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