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CAS No. : | 1015460-59-9 | MDL No. : | MFCD18803689 |
Formula : | C11H7BrN2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | JYFKMOCKASWCPZ-UHFFFAOYSA-N |
M.W : | 247.09 | Pubchem ID : | 71079324 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H317-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 |
---|---|---|
36% | With tetrakis(triphenylphosphine) palladium(0); | Step 3: tert-butyl 17-((5-(5H-pyrido[4,3-b]indol-7-yl)pyridin-2-yl)oxy)-3,6,9,12,15-pentaoxaheptadecan-1-oate To a stirred solution of 7-bromo-5H-pyrido[4,3-b]indole (300 mg, 1.22 mmol), 4,4,4',4',5,5,5',5'-octamethyl-2,2'-bi(1,3,2-dioxaborolane) (620 mg, 2.44 mmol), and potassium acetate (239 mg, 2.44 mmol) in dioxane (5 ml) was added 1,1'-Bis(diphenylphosphino)ferrocene palladium(II)dichloride (176 mg, 0.24 mmol) at room temperature under nitrogen atmosphere, the mixture was degassed with nitrogen three times. The result mixture was stirred at 90° C. overnight. LCMS showed the reaction was complete. To the reaction mixture were added 14-((5-bromopyridin-2-yl)oxy)-3,6,9,12-tetraoxatetradecan-1-ol (930 mg, 1.83 mmol), aqueous sodium carbonate solution (2N, 3.2 ml) and tetrakis(triphenylphosphine)palladium (70 mg, 0.06 mmol); the mixture was degassed with nitrogen three times. The resulting mixture was stirred at 80° C. for 3 hours under nitrogen atmosphere. The reaction mixture was partitioned between ethyl acetate (30 ml) and water (20 ml). The organic layer was collected and the aqueous layer was extracted with ethyl acetate (20 ml). The combined organic layers were washed with brine (30 ml), dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give a crude residue which was purified by silica gel flash chromatography (eluted with 2percent methanol in dichloromethane) to afford tert-butyl 17-((5-(5H-pyrido[4,3-b]indol-7-yl)pyridin-2-yl)oxy)-3,6,9,12,15-pentaoxaheptadecan-1-oate (260 mg, yield 36percent) as grey oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
To a solution of the mixture of regioisomers from Step A above (1.1 g, 4.4 mmol) in xylene (20 mL) was added manganese(IV)-oxide (3.80 g, 40 mmol). The mixture was stirred at 110 C (internal temperature) overnight. The solid material (Mn02) was filtered off through a paper filter, and the solvents were removed under reduced pressure. The residue was purified on HP-Sil cartridges, by employing a dichloromethane/methanol gradient (100/0 -> 90/10) to obtain a mixture of regioisomers (0.47 g, 43%) (0148) MS (ESI): m/z = 247.19/249.18 [M+H]+ |
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