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CAS No. : | 22536-67-0 | MDL No. : | MFCD00673131 |
Formula : | C4H2Cl2N2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | CEJAHXLRNZJPQH-UHFFFAOYSA-N |
M.W : | 148.98 | Pubchem ID : | 590641 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P301+P312-P302+P352-P304+P340-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
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 |
---|---|---|
With [1,1'-bis(diphenylphosphino)ferrocene]nickel(II) chloride; In tetrahydrofuran;Inert atmosphere; Reflux; | To a solution of 2,5-dichloropyrimidine (5 mmol) and Ni(dppf)Cl2 (0.25 mmol) in ether (30 mL) was added MeMgBr (6 mmol, 1M in THF) dropwise under nitrogen atmosphere and the resulting mixture was refluxed overnight. After cooling to rt, water (20 mL) was added and the mixture was extracted with ether (3 x 35 mL). The combined organic layers were washed with brine and dried over anhydrous Na2S04. After filtration and concentration, the crude product was purified by column chromatography to give the title compound. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
376 mg | With dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II)*CH2Cl2; sodium carbonate; In 1,4-dioxane; at 80℃; for 6h;Inert atmosphere; | Step A. tert-butyl-4-(5-Chloropyrimidin-2-yl)benzylcarbamate To a 10 mL microwave vial were added 2,5-dichloropyrimidine (285 mg, 1.8 mmol), Pd(dppf)Cl2.DCM (45 mg, 0.05 mmol), <strong>[489446-42-6](4-(((tert-butoxycarbonyl)amino)methyl)phenyl)boronic acid</strong> (419 mg, 1.67 mmol), Na2CO3 (2 mL, 2M) and 1,4-dioxane (7 mL). The vial was flushed with N2 then capped and placed in a heating block and heated at 80 Celsius. After 6 h, the resulting mixture cooled to RT and transferred to a round-bottomed flask and concentrated to dryness. The residue was purified using FCC to provide 376 mg of the title compound. MS (ESI): mass calcd. for C16H18ClN3O2, 319.11; m/z found 320.1 [M+H]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
640 mg | With potassium carbonate; In N,N-dimethyl-formamide; at 100℃; for 8h;Inert atmosphere; | 2,3-Dihydroxybenzonitrile (270 mg, 2 mmol) and 2,5-dichloropyrimidine (655 mg, 4.4 mmol) were combined in N,N-dimethylformamide (6 mL) under a nitrogen atmosphere. Powdered potassium carbonate (1.2 g, 8.8 mmol) was added, and the resulting mixture was heated at 100 °C for 8 h. The reaction mixture was cooled and diluted with water and ethyl acetate. The aqueous layer was separated and extracted with ethyl acetate (3chi). The combined organic layers were washed with brine, dried (MgS04), filtered and concentrated under reduced pressure. The residue was purified by medium pressure liquid chromatography on silica gel, eluted with 0 to 15percent ethyl acetate in hexanes, to yield the title product, a compound of the present invention, as a solid (640 mg). H NMR (400 MHz, CDC13) delta 7.42-7.49 (m, 1H), 7.57 (dd, J=8.31, 1.47 Hz, 1H), 7.65 (dd, J=7.83, 1.96 Hz, 1H), 8.42 (m, 4H). |
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