Xanthene synthesis
- Product Name:Xanthene
- CAS Number:92-83-1
- Molecular formula:C13H10O
- Molecular Weight:182.22
90-47-1
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92-83-1
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Yield:92-83-1 90%
Reaction Conditions:
with sodium bis(2-methoxyethoxy)aluminium dihydride in toluene at 23 - 60; for 3 h;Inert atmosphere;Solvent;Temperature;
Steps:
1
A 50 ml eggplant type flask was charged with a 70 mass% toluene solution of sodium dihydrobis (2-methoxyethoxy) aluminate (Registered trademark: VITRIDE (VITRIDE), manufactured by Bertrass Specialties Incorporated) 3.47 g (12 mmol) Toluene (10 ml) was added to make it under a nitrogen atmosphere, 588 mg (3 mmol) of xanthone (Wako Junyaku reagent grade 1) dissolved in 10 ml of toluene (special grade, Wako Pure Chemical Industries, Ltd.) was added and stirred at room temperature (23 ° C.). after that, This solution was heated to 60 ° C. and heated and stirred for 3 hours. After standing to cool, 10 ml of a 2N sodium hydroxide aqueous solution was added under ice cooling to make it alkaline. The organic phase was separated and the organic phase was washed twice with 10 ml of saturated sodium bicarbonate. After washing, the organic phase was dried with magnesium sulfate and then toluene was distilled off. As a result, A solid (crude xanthene) was obtained as a residue. This crude xanthene was purified by silica gel column chromatography to obtain 492 mg (90% yield) of xanthene
References:
JP2016/160252,2016,A Location in patent:Paragraph 0030; 0031
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13681-19-1
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92-83-1
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$20.00/1g
