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CAS No. : | 914358-73-9 | MDL No. : | MFCD09031418 |
Formula : | C6H7BrN2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | CBAXYISWNGGXOZ-UHFFFAOYSA-N |
M.W : | 187.04 | Pubchem ID : | 21964096 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | 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 |
---|---|---|
50% | With potassium carbonate;(1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; In 1,2-dimethoxyethane; water; at 100℃; for 1.33333h; | Step 4. N-(6-(5-amino-6-methylpyridin-3-yl)benzo[d1thiazol-2-yl)acetamide; 5-bromo-2-methylpyridin-3-amine (224.9 mg, 1.202 mmol), N-(6-(4,4,5,5-tetramethyl-l ,3,2- dioxaborolan-2-yl)benzo[d]thiazol-2-yl)acetamide (413.7 mg, 1.300 mmol), potassium carbonate (549.4 mg, 3.975 mmol), and Pd(dppf)Cl2*DCM complex (108.7 mg, 0.133 mmol) were suspended in DME (5.0 ml) and water (1.25 ml), and the flask was fit with a reflux condensor and argon was bubbled through for about 15 seconds. Then, the flask was placed in a preheated oil bath (100 C) and stirred under argon for 80 minutes. The reaction was cooled to room temperature, and the aqueous phase was removed via pipette. The reaction was then concentrated, treated with MeOH, and filtered. Solid washed with MeOH, water, MeOH, and Et2O. Solid then collected and dried under high vacuum to afford N-(6-(5-amino-6- methylpyridin-3-yl)benzo[d]thiazol-2-yl)acetamide (179.7 mg, 50% yield). MS (ESI pos. ion) m/z: 299. Calculated exact mass for C15Hi4N4OS: 298. |
50% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In 1,4-dioxane; water; at 80℃; for 8h;Inert atmosphere; | A 25 mL flask was charged with A42-2 (318 mg, 1.00 mmol), 5-bromo-2-methylpyridin- 3-amine A42-3 (187 mg, 1.00 mmol), K2C03(345 mg, 2.50 mmol) and Pd(PPh3)4 (90 mg, 0.078 mmol) followed by addition of dioxane/H20 (10 mL/0.5 mL). The equipment was evacuated and refilled with N2 three times. The reaction was carried out at 80 C for 8 h. After cooled to r.t., the resulting precipitate was filtered. The cake was washed with ethyl acetate to give A42-4 as a white solid (150 mg, 50%).1H NMR (400 MHz, DMSO-d<5) delta 8.13 (s, 1H), 8.00 (s, 1H), 7.73 (d, 7 = 8.4 Hz, 1H), 7.58 (d, J = 8.4 Hz, 1H), 7.20 (s, 1H), 5.14 (s, 2H), 2.30 (s, 3H), 2.18 (s, 3H). |
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