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CAS No. : | 16357-59-8 | MDL No. : | MFCD00006703 |
Formula : | C14H17NO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | GKQLYSROISKDLL-UHFFFAOYSA-N |
M.W : | 247.29 | Pubchem ID : | 27833 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P264-P270-P271-P280-P302+P352-P304+P340-P305+P351+P338-P312-P330-P362+P364-P403+P233-P501 | UN#: | N/A |
Hazard Statements: | H315-H319-H335-H302+H312+H332 | 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 |
---|---|---|
In tetrahydrofuran; ethyl acetate; | (1) To a solution of 3-benzyloxy-2-amino-N-methylaniline (500 mg) and <strong>[422-64-0]pentafluoropropionic acid</strong> (395 mg) in tetrahydrofuran (3 ml) was added 2-ethoxy-1-ethoxycarbonyl-1,2-dihydroquinoline (1.35 g), and the mixture was stirred for 4 hours at 50° C. To the mixture was further added 2-ethoxy-1-ethoxycarbonyl-1,2-dihydroquinoline (108 mg), and the mixture was stirred for 20 hours. The reaction mixture was concentrated in vacuo, and the residue was dissolved in ethyl acetate. The organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by silica gel column chromatography to give a residue containing 3-benzyloxy-2-pentafluoropropionamido-N-methylaniline and 4-benzyloxy-2-pentafluoroethyl-1-methyl-1H-benzimidazole. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
36% | In methanol; dichloromethane; at 20℃; | Compound 23 (5.6 g, 18.52 mmol) was dissolved in DCM (118 mL) andmethanol (58.8 mL). Diol24 (2.70 g, 17.64 mmol) and EEDQ (8.72 g, 35.3 mmol) wereadded and the reaction was stirred at rt overnight. The reaction mixture was concentratedand ethyl acetate was added to the residue. The resulting slurry was filtered, washed with ethyl acetate and dried under vacuum/N2 to give compound 25 as a white solid(2.79 g, 36percent yield). 1H NMR (400 MHz, DMSO-d6): 8 9.82 (s, 1H), 8.05, (d, 1H, J =9.2 Hz), 8.01 (d, 1H, J = 7.2 Hz), 7.46 (s, 2H), 6.95 (3, 1H), 5.21-5.12 (m, 2H), 4.47-4.42 (m, 4H), 4.40-4.33 (m, 1H), 4.33-4.24 (m, 1H), 3.58 (s, 3H), 2.33-2.26 (m, 2H),2.16-2.09 (m, 2H), 1.54-1.46 (m, 4H), 1.30 (d, 3H, J = 7.2 Hz), 1.22 (d, 3H, J = 4.4 Hz). LCMS = 2.894 min (8 min method). Mass observed (ESI+): 438.20 (M+H). |