Alternatived Products of [ 1150617-53-0 ]
Product Details of [ 1150617-53-0 ]
CAS No. : | 1150617-53-0 |
MDL No. : | MFCD12024389 |
Formula : |
C7H7BrN2O2
|
Boiling Point : |
- |
Linear Structure Formula : | - |
InChI Key : | - |
M.W : |
231.05
|
Pubchem ID : | - |
Synonyms : |
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Safety of [ 1150617-53-0 ]
Application In Synthesis of [ 1150617-53-0 ]
* 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 [ 1150617-53-0 ]
- 1
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[ 74-89-5 ]
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[ 886762-70-5 ]
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[ 1150617-53-0 ]
Yield | Reaction Conditions | Operation in experiment |
96% |
In ethanol; |
An 8 M methylamine sol. in ethanol (100 ml, 0.8 mol) was added to l-bromo-3-fluoro- 2-nitro-benzene (19.8 g, 90 mmol). The mixture was cooled on a water bath and was stirred overnight at r.t. Then, the solvent was evaporated and the residue was partitioned between water and DCM. The combined organic layers were dried (MgSO4), filtered and concentrated in vacuo. Yield: 20 g of intermediate 17 (96 %), which was used as such in the next step. |
96% |
In ethanol; at 20℃; |
Example A4 a) Preparation of intermediate 10A 8 M methylamine sol. in EtOH (100 ml, 0.8 mol) was added to l-bromo-3-fluoro-2- nitro-benzene (19.8 g, 90 mmol), cooled on a water bath. The r.m. was stirred at r.t. overnight. Then, the solvent was evaporated and the residue was partitioned between water and DCM. The combined organic layers were dried (MgSO4), filtered and concentrated in vacuo. Yield: 20 g of intermediate 10 (96 %), which was used as such in the next reaction step. |
|
In tetrahydrofuran; at 80℃; for 2h; |
A solution of i-bromo-3-fluoro-2-nitrobenzene(iO g, 45.6 mmol) in NH2CH3 inTHF (2 M, 100 ml) was stirred at 80C for 2 hr. The reaction mixture was concentrated undervacuumto give 3-bromo-N-methyl-2-nitrobenzenamine. LCMS (ESI) calc?d forC7H7BrN2O2[M+ i]: 231, found [M+i]: 231, ?H NMR (CDC13, 400 MHZ): 7.21-7.16 (m, iH), 6.97 (d, J 7.6Hz, iH), 6.76 (d, J= 7.6 Hz, iH), 2.94 (s, 3H). |
Reference:
[1]Patent: WO2010/89292,2010,A1 .Location in patent: Page/Page column 67
[2]Patent: WO2010/94647,2010,A1 .Location in patent: Page/Page column 64
[3]Journal of Medicinal Chemistry,2012,vol. 55,p. 9089 - 9106,18
[4]Patent: WO2016/206101,2016,A1 .Location in patent: Page/Page column 78
[5]Journal of Medicinal Chemistry,2019,vol. 62,p. 234 - 246