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Chemical Structure| 701298-37-5 Chemical Structure| 701298-37-5

Structure of 701298-37-5

Chemical Structure| 701298-37-5

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Product Details of [ 701298-37-5 ]

CAS No. :701298-37-5
Formula : C12H24N2O3
M.W : 244.33
SMILES Code : O=C(N1CCC(NCCO)CC1)OC(C)(C)C
MDL No. :MFCD12106425

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Application In Synthesis of [ 701298-37-5 ]

* 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 [ 701298-37-5 ]

[ 701298-37-5 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 701298-37-5 ]
  • [ 90176-80-0 ]
  • [ 710978-91-9 ]
YieldReaction ConditionsOperation in experiment
With sodium tris(acetoxy)borohydride; In DMF (N,N-dimethyl-formamide); 1,2-dichloro-ethane; at 20℃; for 16h; To a solution of amine prepared in intial step (2. 0g, 8. 19MMOL, L. Oeq) in dichloroethane (20 ml) was added the 4-fluoro, 2- (trifluoromethyl) benzaldehyde (2.34g, 12.2mmol, 1. 5eq). To this was added sodium triacetoxyborohydride (2.58g, 12. 2MMOL, 1. 5eq.) in DMF (lml). This mixture was left to stir under nitrogen, at room temperature for 16h. The reaction was worked up by addition of water (10 ml). The mixture was stirred vigorously for several minutes. The chlorinated organic layer was then run through a hydrophobic frit to remove water. The resulting organic solution was diluted with methanol (10 ml) and loaded onto an SCX-2 (lOg) column. The column was washed with methanol (50 ml) then basic material eluted with 2N ammonia in methanol. The ammonia/methanol solution was concentrated in vacuo to give an oil. This was further purified using ISCO chromatography, eluting with 0-40% ethyl acetate: iso-hexane ramp over 40 min to give the desired compound (0. 173G), which was taken onto the next step. To a solution of this oil (L. Oeq) in dichloromethane (10 ML) was added trifluoroacetic acid (TFA) (15EQ). The solution was stirred at room temperature for 4h. Solvent and TFA were removed in vacuo. The resulting oil was taken up in methanol and loaded onto an SCX-2 (10 g) column. The column was washed with methanol (50 ml). Basic material was then eluted using 2N ammonia in methanol (50 ml). Removal of solvent from the ammonia/methanol mixture under vacuum, gave the desired compound as an oil. The oil was taken up in diethyl ether. To this solution was added a solution OF FUMARIC acid (LEQ) in hot methanol and then cooled. The resulting precipitate was collected by filtration to give the title compound as a white solid (0.43g) ; IHNMR (MEOD) 6= 8.10- 8.0 (1H, m), 7.45-7. 33 (2H, m), 6.69 (2H, s), 3.91 (2H, s), 3.59-3. 41 (4H, m), 3.30-3. 21 (1H, s), 3.10-2. 81 (3H, m), 2.75-2. 68 (2H, m), 2.15 (2H, brd), 1.87-1. 70 (2H, m).
 

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