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2-(2,3-Dichlorophenyl)ethyl methansulfonate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
100%
a. 2-(2,3-Dichlorophenyl)ethyl methansulfonate Using the method of Example 1a, but substituting <strong>[114686-85-0]2,3-dichlorphenethyl alcohol</strong> for 3-methoxyphenethyl alcohol and reacting at 0 C. for 4 hr, the title product was obtained as a yellow oil in 100% yield.
100%
a. 2-(2,3-Dichlorophenyl)ethyl methansulfonate Using the method of Example 1a, but substituting <strong>[114686-85-0]2,3-dichlorphenethyl alcohol</strong> for 3-methoxyphenethyl alcohol and reacting at 0C for 4 hr, the title product was obtained as a yellow oil in 100% yield.
With sodium hydrogencarbonate; Dess-Martin periodane; In dichloromethane; water; for 1h;
A mixture of <strong>[114686-85-0]2-(2,3-dichlorophenyl)ethanol</strong> (0.50 g), NaHCO3 (0.438 g) and Dess-Martin periodinane (1.22 g) in dichloromethane (10 mL) and water (46 mL) was stirred for 1 hour. The mixture was quenched with aqueous NaHCO3 and saturated aqueous Na2S2O3 and extracted with dichloromethane. The extract was dried (Na2SO4), filtered and concentrated. The concentrate was purified on silica gel with an Intelliflash-280 purification system with hexanes/ethyl acetate.
General procedure: The starting material, 2-(3,4-dimethoxyphenyl)-ethan-1-ol (521 mg, 2.86 mmol, 1.0 equiv) was dissolved in dichloromethane (20 mL) and imidazole (583 mg, 8.58 mmol, 3.0 equiv) was added. The mixture was stirred for 5 minutes. tert-Butyldimethylsilyl chloride (518 mg, 3.43 mmol, 1.2 equiv) was added and the reaction mixture was stirred at room temperature for 1 hr. Water (20 mL) and dichloromethane (20 mL) were added and the mixture was shaken in a separating funnel. The aqueous layer was separated and washed with dichloromethane (2 x 5 mL). The combined organic layers were washed with water (20 mL), brine (20 mL) and dried over MgSO4. Following filtration, the solvent was removed under reduced pressure. The crude material was purified by column chromatography on silica gel (eluting with a gradient from petroleum ether to 1:1 petroleum ether : ether) to afford 820mg of 1a (97%).
With toluene-4-sulfonic acid; In methanol; dichloromethane; at 20 - 25℃; for 0.333333h;Flow reactor;
General procedure: The system (Figure 4) was primed with solvent (DCM and 0.3 M aqueous NaOH) prior to the introduction of the substrates. Substrates were present as 0.034 M solutions (20 mL) in glass vials. These were placed in a square 4 x 4 rack. Following initiation of the computer-vision system (and checking to make sure the aqueous-out tap was opening/closing properly), activation of the autosampler/liquid-handling schedule was initiated by pressing ?s? on the computer keyboard. The outlet of the flow stream for each product was then collected until the autosampler moved to the waste position between each run. 5 mL of substrate was taken up during each run, 4 mL of which entered the holding loop (the line between the autosampler and 3-way-valve 1 was 1 mL in volume). Outlet collection flasks were changed manually. The products were isolated by removing solvent under reduced pressure.
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