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CAS No. : | 263400-88-0 | MDL No. : | MFCD22124592 |
Formula : | C11H16O5S2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | AXUFUWARAAYMCG-UHFFFAOYSA-N |
M.W : | 292.37 | Pubchem ID : | 22732325 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-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 |
---|---|---|
85% | With potassium carbonate; In N,N-dimethyl-formamide; at 90℃; for 12h; | Reference Example 17; {2' , 3' ,5' , 6'-tetramethyl-4' - [3- (methylsulfonyl)propoxy]biphenyl-3-yl}methanol; To a solution of 3'- (hydroxymethyl) -2, 3, 5, 6- tetramethylbiphenyl-4-ol (0.616 g, 2.40 mmol) and 3- (methylsulfonyl) propyl 4-methylbenzenesulfonate (1.05 g, 3.60 mmol) in N,N-dimethylformamide (5 mL) was added potassium carbonate (0.597 g, 4.32 mmol), and the mixture was stirred at 9O0C for 12 hr under nitrogen atmosphere. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed successively with 1 M aqueous sodium hydroxide solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate :hexane = 40:60 - 80:20), and the obtained crystals were recrystallized from heptane-ethyl acetate to give the title compound (0.577 g, yield 85%) as colorless crystals, melting point 132-134C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88% | With potassium carbonate; In N,N-dimethyl-formamide; at 90℃; for 24h; | Weigh YZ-2 (2·26g, 10mmol), YZ-1 (3·51g, 12mmol), potassium carbonate (1·8g, 13mmol), was dissolvedIn 20ml N,Nu-dimethylformamide, and the reaction was stirred at 90C in an oil bath for 24 hours, until the reaction was complete feed YZ-2. 150mL was added in the reaction system was diluted with ethyl acetate, washed successively with water, saturated brine, dried over anhydrous sodium sulfate,Filtered, and concentrated to give the crude product was purified by flash column chromatography (30% ethyl acetate / petroleum ether) to give the product YZ-3 (3.05g), yield 88%. |
78% | With potassium carbonate; In N,N-dimethyl-formamide; at 90℃; for 24h;Inert atmosphere; | To a solution of product 20 (1.36g, 6.00mmol) and product 19 (2.1 lg, 7.20mmol) in N, N-dimethylformamide (12mL) was added potassium carbonate (1.08g, 7.80mmol), and the mixture was stirred at 90 C for 24 hr under nitrogen atmosphere .Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed successively with 1 M aqueous sodium hydroxide solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (ethyl acetate: hexane = 40:60-80:20), and the obtained crystals were recrystallized from heptane-ethyl acetate to give a colorless solid product 21 (1.61g, yield 78%). |
77% | With potassium carbonate; In N,N-dimethyl-formamide; at 90℃; for 24h; | Reference Example 18; 2' , 6' -dimethyl-4f - [3- (methylsulfonyl)propoxy]biphenyl-3-carbaldehyde; <n="82"/>To a solution of 4'-hydroxy-2' , 6'-dimethylbiphenyl-3- carbaldehyde (2.26 g, 10.0 itimol) and 3- (methylsulfonyl) propyl 4-methylbenzenesulfonate (3.51 g, 12.0 rartiol) in N,N- dimethylformamide (20 mL) was added potassium carbonate (1.80 g, 13.0 mmol) , and the mixture was stirred at 900C for 24 hr under nitrogen atmosphere. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed successively with 1 M aqueous sodium hydroxide solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate :hexane = 40:60 - 80:20), and the obtained crystals were recrystallized from heptane-ethyl acetate to give the title compound (2.68 g, yield 77%) as colorless crystals.MS m/z 347 (M + H)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With potassium carbonate; In N,N-dimethyl-formamide; at 90℃; for 24h; | Reference Example 26; 3'-fluoro-2' , 6' -dimethyl-4' - [3- (methylsulfonyl) propoxy] biphenyl-3-carbaldehyde; To a solution of 3' -fluoro-4'-hydroxy-2' , 6' - dimethylbiphenyl-3-carbaldehyde (2.44 g, 10.0 mmol) and 3- (methylsulfonyl) propyl 4-methylbenzenesulfonate (3.51 g, 12.0 mmol) in N,N-dimethylformamide (20 mL) was added potassium carbonate (1.80 g, 13.0 mmol), and the mixture was stirred at 900C for 24 hr under nitrogen atmosphere. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed successively with 1 M aqueous sodium hydroxide solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced <n="87"/>pressure. The residue was purified by silica gel column chromatography (ethyl acetate rhexane = 40:60 - 80:20), and the obtained crystals were recrystallized from heptane-ethyl acetate to give the title compound (3.45 g, yield 95%) as colorless crystals . MS m/z 365 (M + H)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With potassium carbonate; In N,N-dimethyl-formamide; at 90℃; for 21h; | Reference Example 37; {3'- (hydroxymethyl) -6-methyl-4- [3- (methylsulfonyl) propoxy]biphenyl-2-yl }methyl acetate; To a solution of [4-hydroxy-3' - (hydroxymethyl) -6- methylbiphenyl-2-yl]methyl acetate (1.02 g, 3.56 mmol) and 3- (methylsulfonyl) propyl 4-methylbenzenesulfonate (1.25 g, 4.27 mmol) in N,N-dimethylformamide (10 mL) was added potassium carbonate (0.640 g, 4.32 mmol), and the mixture was stirred at 900C for 21 hr under nitrogen atmosphere. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate :hexane = 50:50 - 100:0) to give the title compound (0.87 g, yield 60%) as a colorless oil.1H NMR (CDCl3) delta: 1.81(1H, t, J=6.0Hz), 2.01(3H, s) , 2.03(3H, <n="93"/>. s) , 2.31-2 .43 (2H, m) , 2.97 (3H, s) , 3.24-3.32 (2H, m) , 4 .16 (2H, t, J=5.7Hz ) , 4 .72 ( 2H, d, J=6. 0Hz) , 4 .76 (2H, s) , 6.78 ( IH, d, J=2.5Hz) , 6. 83 ( IH, d, J=2 . 5Hz) , 7 . 05-7.10 ( 1H, m) , 7. 15 ( 1H, s ) , 7 . 32-7 .43 ( 2H, m) . |
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