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CAS No. : | 10287-53-3 | MDL No. : | MFCD00009115 |
Formula : | C11H15NO2 | Boiling Point : | - |
Linear Structure Formula : | C6H4[N(CH3)2](COOC2H5) | InChI Key : | FZUGPQWGEGAKET-UHFFFAOYSA-N |
M.W : | 193.24 | Pubchem ID : | 25127 |
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 |
---|---|---|
With hydrogenchloride; In hexane; tert-butyl methyl ether; ethyl acetate; | EXAMPLE 8 Preparation of (3beta,5Z,7E)-9,10-Secocholesta-5,7,10(19),16-tetraen-23-yne-3,25-diol Diacetate A solution of 16.4 g (34.3 mmol) (3beta)-cholesta-5,7,16-trien-23-yne-3,25-diol diacetate and 1.64 g ethyl 4-dimethylaminobenzoate in 1.7 L of tert-butyl methyl ether at -20 C. was irradiated with a 450 W medium pressure lamp through a quartz immersion well. During the photolysis, the arc housing was constantly purged with a slow current of nitrogen. After 8 hr of irradiation at 0 to -20 C., a uranium filter was inserted in the arc housing, and then 66 mg of <strong>[784-04-3]9-acetylanthracene</strong> was added to the solution. After 1 hr 45 min of irradiation through the filter at 0 to -20 C., the solution was allowed to warm to room temperature overnight, and then washed four times with a total of 400 mL of 3N HCl. The organic layer was then washed with 200 mL of saturated aqueous NaHCO3 and dried over Na2 SO4. The solution was concentrated to dryness. Then the residual oil was purified by chromatography on silica gel, eluding with 3 L of 7% ethyl acetate in hexane. After discarding about 0.8 L of eluent, the desired fractions were combined and concentrated to give about 13 g of a clear oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In methanol; hexane; tert-butyl methyl ether; | EXAMPLE 11 (1alpha,3beta,5Z,7E)-9,10-Secocholesta-5,7,10(19),16-tetraen-23-yne-1,3,25-triol A 2-L photoreactor was charged with 10 g (24.4 mmol) of (1alpha,3beta)-cholesta-5,7,16-trien-23-yne-1,3,25-triol, 1 g of ethyl 4-dimethylaminobenzoate, 1.45 L of methanol, and 250 mL of tert-butyl methyl ether. After cooling to -10 C., the solution was irradiated with a 450 W medium pressure Hg lamp at -10 to -30 C. for 7.5 hr. A uranium filter was inserted to the arc housing, and 50 mg of <strong>[784-04-3]9-acetylanthracene</strong> in 2 mL of tert-butyl methyl ether was added. The mixture was irradiated with the same lamp through the filter at -10 to -30 C. for 1.5 hr. The mixture was allowed to warm to from temperature overnight. The solution was concentrated to about 1 L, and then refluxed for 4 hr. The mixture was allowed to cool to room temperature overnight, and concentrated to dryness. The residue was purified repeatedly by chromatography on silica gel, eluding with 60% EtOAc in hexane. The desired fractions were combined and concentrated to dryness. The residue was then recrystallized from aqueous methanol to afford (1alpha,3beta,5Z,7E)-9,10-secocholesta-5,7,10(19),16-tetraen-23-yne-1,3,25-triol. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: A flame-dried Schlenk test tubewith a magnetic stirring bar was charged with NaH (60% suspension in mineral oil) in dry THF (4 mL) at room temperature under N2 atmosphere.4-(Dimethylamino)acetophenone (250 mg, 1.53 mmol) was then added and the mixture was stirred for 10 min, followed by the addition of ethyl benzoate (340 mg, 1.76 mmol). The reaction mixture was refluxed for 8 h to give a viscous yellow suspension. The reaction was quenched with ice water(50 mL), and the pH was adjusted to 5-7 with hydrochloric acid. The light yellow precipitates formed were quickly filtrated and washed with cold water. The crude product was recrystallized with ethanol / water = 1:1 to afford the pure dibenzoylmethane derivative as light yellow needles.2 For the precursor of 3, the reaction mixture was extracted with ethyl acetate (20 mL × 3). The combined organic phase was washed with water, dried over anhydrous Na2SO4 and filtered. After removal of the volatile solvent by rotary evaporation, the crude product was obtained by flash chromatography. Recrystallization with ethanol / water = 1:1 afforded the purecompound as a yellow crystal.3 |
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