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CAS No. : | 134419-59-3 | MDL No. : | MFCD11505063 |
Formula : | C6H12O4S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | GSEZHCLWHDZJAB-UHFFFAOYSA-N |
M.W : | 180.22 | Pubchem ID : | 11344352 |
Synonyms : |
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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 |
---|---|---|
100% | With potassium carbonate; In acetonitrile; for 20h;Heating / reflux; | Methyl <strong>[89942-77-8]3-hydroxy-2-nitrobenzoate</strong> (95 g, 0.52 mol), tetrahydro-2H-pyran-4-yl methanesulfonate (234 g, 1.3 mol) and K2CO3 (358 g, 2.6 mol) was suspend in MeCN (2 L). The mixture was heated at reflux for 20 h. TLC (petroleum ether: ethyl acetate = 1:1) showed the reaction was complete. The mixture was filtered; the filtrate was concentrated in vacuo. The residue was purified by chromatography (petroleum ether: ethyl acetate=10:1 , 5:1 , 2:1) to give the title compound (200 g 100%) as a yellow oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
19% | With caesium carbonate; In N,N-dimethyl-formamide; at 80℃; | A vial was charged with <strong>[5932-27-4]ethyl-1H-pyrazole-3-carboxylate</strong> (3.74 g, 26.7 mmol), the crude methanesulfonic acid tetrahydro-pyran-4-yl ester (29.4 mmol), Cs2CO3 (17.4 g, 53.4 mmol), and DMF (100 mL). The reaction mixture was heated to 80° C. and stirred overnight. The reaction was then partitioned between CH2Cl2 (250 mL) and water (250 mL), and the organic layer was washed with water (5*250 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude product containing 2 regioisomers was purified via flash chromatography on silica gel (95:5-50:50 hexanes:EtOAc) and the later eluting isomer was isolated. This was purified on silica gel a second time (85:15-60:40 hexanes:EtOAc) to give the pure desired product (1.14 g, 19percent). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
15% | In N,N-dimethyl-formamide; at 80℃; for 12h; | To a solution of <strong>[1086391-06-1]methyl 3-bromo-1H-indazole-5-carboxylate</strong> (2.0 g,7.8 mmol)and5 Cs2C03 (5.1 g,15.7 mmol)in DMF (10 mL)was added tetrahydro-2H-pyran-4-ylmethanesulfonate (2.1 g,11.7 mmol). The reaction was heated to 80 C for 12 h. After coolingto room temperature,the reaction was concentrated in vacuo. EtOAc (80 mL)was added andwashed with water (100 mL x 3),brine (100 mL). The organic layer was dried over anhydrousNa2S04,filtered and concentrated in vacuo. The crude residue was purified by silica gel10 chromatography (petroleum ether/EtOAc = 10:1)to give the title compound (400 mg,15%)as ayellow solid. 1H NMR (400 MHz,DMSO-d6)8 8.39 (s,1H),8.12- 8.09 (m,1H),7.47 (d,J =8.8 Hz,1H),4.67- 4.59 (m,1H),4.20- 4.16 (m,2H),3.97 (s,3H),3.67- 3.55 (m,2H),2.47-2.36 (m,2H),2.00- 1.96 (m,2H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate; In N,N-dimethyl-formamide; at 100.0℃; for 18.0h; | Step2: 5-Bromo-3-chloro-2-((tetrahydro-2H-pyran-4-yl)oxy)pyridine[254][255]Potassium carbonate (2.0 eq.) was added to a solution of tetrahydro-2H-pyran-4-yl methanesulfonate (1.2 eq.) and 5-bromo-3-chloropyridine-1-ol (1.0 eq.) in N,N-dimethylformamide (0.2 M). The reaction mixture was stirred at 100 for 18 h. The reaction mixture was allowed to reach room temperature, diluted with ethyl acetate and washed with water. The organic layer was washed with brine, dried over magnesium sulfate, filtered and concentrated. The resultant residue was purified by flash column chromatography on silica gel to afford 5-bromo-3-chloro-2-((tetrahydro-2H-pyran-4-yl) oxy) pyridine. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
37.33% | With caesium carbonate; In N,N-dimethyl-formamide; at 60℃; for 16h; | To the stirred solution of tetrahydropyran-4-yl methanesulfonate 17-2 (675.22 mg, 3.75 mmol) in DMF (5 rnL) were added cesium carbonate (3.05 g, 9.37 mmol) and IH-<strong>[35344-95-7]pyrazole-4-carbaldehyde</strong> 17-1 (300 mg, 3.12 mmol). The reaction mixture was heated at 60C for 16 hours and was then quenched with cold water. The organic layer was extracted with ethyl acetate, washed with saturated solution of sodium bicarbonate, dried over sodium sulfate and concentrated under reduced pressure to afford crude which was purified by column chromatography to afford l-tetrahydropyran-4- yl<strong>[35344-95-7]pyrazole-4-carbaldehyde</strong> 17-3 (210 mg, 1.17 mmol, 37.33% yield) as gummy solid. LC MS:ES+ 181.1. |
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