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CAS No. : | 2942-13-4 | MDL No. : | MFCD01961206 |
Formula : | C8H7NOS | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | AHOIGFLSEXUWNV-UHFFFAOYSA-N |
M.W : | 165.21 | Pubchem ID : | 350186 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-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 |
---|---|---|
51% | With tert.-butylhydroperoxide; copper dichloride; In water; at 80.0℃; for 24.5h;Inert atmosphere; Schlenk technique; | General procedure: A 25 mL reaction vessel was charged with benzothiazole 1 (1.86 mmol, 1.1 equiv), aldehyde 2 (1.69 mmol), CuCl2 (0.51mmol, 0.3 equiv), and tert-butylhydroperoxide (2.36 mmol, 1.4 equiv, 70% aqueous solution) under nitrogen. The reactionmixture was stirred in an ice bath for 30 min, and then stirred at 80C for 24 h. After cooling to room temperature, the mixture was purified by column chromatography using silica gel (petroleum ether/ethyl acetate) to afford the products 3. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
7.6% | With bis(tri-t-butylphosphine)palladium(0); caesium carbonate; copper(I) bromide; In N,N-dimethyl-formamide; at 150℃; for 16h;Molecular sieve; Inert atmosphere; | Step 1, Method 2: 4-(6-Methoxy-l,3-benzothiazol-2-yl)pyridine-3-carbonitrile[0147] To a degassed, stirred mixture of 6-methoxy-l,3-benzothiazole (324 mg, 1.96 mmol, as described in Tetrahedron 53, (1997), 17029-17038), 4-bromopyridine-3- carbonitrile (436 mg, 2.38 mmol), copper(I) bromide (59 mg, 0.41 mmol), caesium carbonate (642 mg, 1.97 mmol) and molecular sieves in dry N,N-dimethylformamide (16 mL) was added palladium - tri-tert-butylphosphane (1 :2) (49 mg, 0.1 mmol). The mixture was degassed before heating to 150 C under nitrogen gas for 16 hours. The cooled reaction mixture was filtered through 'Kieselguhr' and washed with ethyl acetate (4 x 10 mL). A 1 : 1 mixture of water and brine (100 mL) was added to the filtrate and the two-phase system filtered and washed with ethyl acetate (20 mL). The aqueous layer was extracted with ethyl acetate (2 x 20 mL). The combined organic layers were washed with a 1 : 1 mixture of water and brine (3 x 80 mL). The second aqueous washings were back extracted with ethyl acetate (10 mL); the organic layers were combined and washed with brine (50 mL), dried over magnesium sulphate, filtered and concentrated. Crude material was purified by FCC (silica, 0-80% ethyl acetate in heptane), sonicated in tert-butyl methyl ether (2 mL), filtered, washed with tert-butyl methyl ether (1 x 2 mL and 2 x 1 mL) and dried to give the title compound 40 mg (7.6% yield) as a beige solid.Example 1, Method 2: 4-(6-Methoxy-l,3-benzothiazol-2-yl)pyridine-3- carbonitrile[0148] 5H MR (500 MHz, DMSO) 9.20 (s, 1 H) 8.99 (d, J=5.20 Hz, 1 H) 8.15 (d, J=5.36 Hz, 1 H) 8.08 (d, J=8.98 Hz, 1 H) 7.88 (d, J=2.36 Hz, 1 H) 7.25(dd, J=8.99, 2.36 Hz, 1 H) 3.89 (s, 3 H). Tr(METCR1416) = 4.02 min, (ES+) (M+H)+268. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | In the reaction flask, Under argon, a catalyst (9.9 mg, 0.025 mmol, 5 mol%), potassium tert-butoxide (0.0672 g, 0.6 mmol) DMF (3.0 mL), 6-methoxybenzothiazole (82.5 mg, 0.5 mmol), access to carbon dioxide gas, The reaction was stirred at 80 C for 18 hours under normal pressure. Cooled to 65 C, methyl iodide (93 mul, 1.5 mmol) was added, The reaction was stirred at 65 C for 1 hour. Cooled to room temperature, the reaction was terminated with deionized water, The reaction product was extracted with ethyl acetate and purified by column chromatography (Using a mixed solvent of ethyl acetate / petroleum ether in a volume ratio of 1:10 as a developing solvent) The yield was 82%. |
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