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[ CAS No. 2251-78-7 ] {[proInfo.proName]}

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Chemical Structure| 2251-78-7
Chemical Structure| 2251-78-7
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Product Details of [ 2251-78-7 ]

CAS No. :2251-78-7 MDL No. :
Formula : C8H5F3N2O Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 202.13 Pubchem ID :-
Synonyms :

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Precautionary Statements: UN#:
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* 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 [ 2251-78-7 ]

[ 2251-78-7 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 2251-78-7 ]
  • [ 1075753-27-3 ]
YieldReaction ConditionsOperation in experiment
1.1 g With trichlorophosphate; at 120℃; for 2h; Step B: 2-Chloro-4-(trifluoromethy)l- 1 H-benzo [d] imidazole To 4-(trifluoromethyl)-lH-benzo[d]imidazol-2(3H)-one (1.7 g, 8.4 mmol) from example 11, step A, was added POCb (7.8 ml, 84 mmol). The reaction mixture was stirred at 120C for 2 hours and then cooled to room temperature. The mixture was stirred overnight and the excess POCb was removed in vacuo. The remaining crude material was cooled in an ice bath and ethyl acetate was added with very small amounts of water. The resulting mixture was then slowly poured into an ice cooled flask containing water. The flask was allowed to warm to room temperature and the mixture was then neutralized with sat'd NaHCCb. The organics were separated, dried with MgS04, filtered and the solvent was removed to yield a brown powder. The crude material was purified by chromatography (Biotage) to yield 2-chloro-4-(trifluoromethyl)- 1 H-benzo [d] imidazole (1.1 g, 5 mmol, 59 % yield) as a powder.
Reference： [1]Bioorganic and Medicinal Chemistry Letters,2008,vol. 18,p. 5010 - 5014
[2]Patent: WO2016/73407,2016,A1 .Location in patent: Page/Page column 59
  • 2
  • [ 360-60-1 ]
  • [ 530-62-1 ]
  • [ 2251-78-7 ]
YieldReaction ConditionsOperation in experiment
In tetrahydrofuran; at 20℃; Step A: 4-(Trifluoromethyl)-l ol-2(3H)-one To a solution of 3-(trifluoromethyl)benzene-l,2-diamine (2 g, 11 mmol) in anhydrous THF (60 mL) was added CDI (3.7 g, 23 mmol). The reaction mixture was stirred at room temperature overnight. The solvent was removed under reduced pressure and the residue chromatographed (Biotage) to yield a cream colored powder, 4- (trifluoromethyl)-lH4oenzo[d]imidazol-2(3H)-one (1.8 g, 8.9 mmol, 78 percent yield), which was carried on to the next step without any further purification. NMR (500MHz, DMSO-ck) delta 1 1.40 - 10.83 (m, 2H), 7.27 - 7.01 (m, 3H). MS (LC/MS) R.T. = 4.88; [M+l]+ = 203.03.
Reference： [1]Patent: WO2016/73407,2016,A1 .Location in patent: Page/Page column 58-59

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