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CAS No. : | 241479-67-4 | MDL No. : | |
Formula : | C22H17F2N5OS | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | DDFOUSQFMYRUQK-RCDICMHDSA-N |
M.W : | 437.47 | Pubchem ID : | 6918485 |
Synonyms : |
BAL-4815;RO-0094815;trade name Cresemba.;BAL-8557-002
|
Chemical Name : | 4-[2-[(1R,2R)-2-(2,5-Difluorophenyl)-2-hydroxy-1-methyl-3-(1H-1,2,4-triazol-1-yl)propyl]-4-thiazolyl]benzonitrile |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | sodium iodide; In acetonitrile; at 20 - 80℃; for 9h; | A solution of 1-[3-[4-(4-cyano-phenyl)-thiazol-2-yl]-2-(2,5-difluoro-phenyl)-2-hydroxy-butyl-1H-[1,2,4]triazol (200 mg, 0.457 mmol), sodium iodide (6.8 mg 0.045 mmol) and acetic acid 2-(chloromethoxycarbonyl-methyl-amino)-benzyl ester 150 mg, 0.552 mmol) was stirred for 6 h at ambient temperature and then at 80° C. for 3 h under Ar atmosphere. The reaction mixture was concentrated under reduced pressure and the resulting material was eluted on a column of silica gel (Kusano Si-5, eluent dichloromethane:methanol=20:1). The fractions containing the product were concentrated under reduced pressure giving the title compound a) as colorless amorphous (204.5 mg, 63percent). 1H-NMR (270 MHz, DMSO-d6): delta 1.20 (3H, d, J=6.9), 1.99 (3H, s), 3.12 (2.4H, s), 3.15 (0.6H, s), 4.15 (1H, q, J=7.3), 4.79-4.91 (3H, m), 5.09 (1H, d, J=14.8), 5.76 (1H, s), 5.90-6.10 (1.6H, m), 6.17 (0.4H, br.s), 6.61-6.66 (1H, m), 7.05-7.15 (1H, m), 7.26-7.44 (6H, m), 7.91-7.96 (2H, m), 8.20-8.24 (2H, m),8.49 (1H, s), 9.01 (0.8H, br.d, J=3.6), 9.12 (0.2H, br.s), 10.16 (0.8H, br.d, J=4.9), 10.27 (0.2H, br.s); FAB-MS: 673 (M-Cl)+; Ratio of Retention Time in HPLC: 1.79 (see Example D). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | sodium iodide; In acetonitrile; at 70℃; | To a solution of [N-methyl-N-2-((tert-butoxycarbonylisopropylamino)methyl)phenyl]carbamic acid 1-chloro-ethyl ester (143 mg, 0.342 mmol) in acetonitrile (1 ml) was added the azole compound (163 mg, 0.372 mmol) and catalytic amount of sodium iodide at 70° C. After stirring overnight, the solvent was removed and extracted with ethyl acetate. The organic phase was washed with water and brine. The solvent was removed in vacuo. The residue was purified by column chromatography (ethyl acetate to 10percent methanel-dichloromethane) to afford 1-[[N-methyl-N-2-(t-butoxycarbonyl-isopropylaminomethyl)phenyl]carbamoyloxy]ethyl-1-[(2R,3R)-2-(2,5-difluorophenyl)-2-hydroxy-3-[4-(4-cyano-phenyl)thiazol-2-yl]butyl]-1H-[1,2,4]triazol-4-ium chloride (155 mg, 0.189 mmol, 51percent) as off-white amorphous. |