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CAS No. : | 138642-47-4 | MDL No. : | MFCD01861260 |
Formula : | C8H6BrNO | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | ZQONVYONOASKIY-UHFFFAOYSA-N |
M.W : | 212.04 | Pubchem ID : | 21784096 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P305+P351+P338-P330-P332+P313-P337+P313-P362-P403+P233-P405-P501 | UN#: | N/A |
Hazard Statements: | H302-H312-H315-H319-H332-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% | Step A: 1-(2-Bromo-5-methoxyphenyl)methanamine 2-Bromo-5-methoxybenzonitrile (10.0 g, 47.2 mmol) was dissolved in dry tetrahydrofuran (100 mL) in a flame-dried flask and cooled in an ice bath. A solution of borane in tetrahydrofuran (75 mL, 75 mmol, 1.0 M) was added dropwise over a period of 30 minutes. The reaction mixture was stirred overnight at rt, then quenched slowly with ice water and Na2CO3 (saturated aqueous solution). After removal of THF, the residue was extracted with large amounts of EtOAc three times. The combined organic layers were washed with water, dried, and concentrated to give the crude, which was purified by silica gel column chromatography to give the desired product as a white powder (3.65 g, 36%). LCMS for C8H10BrNO (M+H)+: m/z=216.9, 219.0. | |
With ammonia; hydrogen;nickel; under 25858.1 Torr; | In Scheme 75, a nitrile of formula (6) is reduced with hydrogen gas at 500 pounds-per-square-inch ("psi") pressure in the presence of a catalyst such as Raney nickel in methanol and ammonia, for example, to give the aminomethyl (7). Compound (7) may be alkylated with a compound of formula [R2-X] as described above in Scheme 74 to give compound (8). Compound (8) may be carbonylated in a manner similar to that described above for Scheme 74 to give an intermediate which cyclizes in situ to a compound (9). Compound (9) may be converted to compound (10) by demethylation with [BORONTRIBROMIDE] in dichloromethane followed by acylation of the intermediate phenol derivative with trifluoromethanesulfonic acid anhydride ("TFMSAA"). Compound (10) may be converted to compound (11) in a manner similar to that described above for Scheme 74. Alternatively, compound (11) may be converted to compound (12) by carbonylation in a manner similar to that described above for Scheme 74. Compound (12) may be converted to amide (13) in a manner similar to that described above for Scheme 74. |
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