1,4,5,8,9,10-Hexahydroanthracene synthesis
- Product Name:1,4,5,8,9,10-Hexahydroanthracene
- CAS Number:5910-28-1
- Molecular formula:C14H16
- Molecular Weight:184.28
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Yield:5910-28-1 91%
Reaction Conditions:
with lithium;tert-butyl alcohol in tetrahydrofuran at -10 - 0;Inert atmosphere;
Steps:
5 Example 5
In a 250ml three-neck flask, vent nitrogen, add 8.9g (50.0mmol) of anthracene, 100ml of tetrahydrofuran and 44.5g (600.0mmol) of tert-butanol, stir mechanically, cool down in a low-temperature coolant circulating pump, and install a thermometer to keep the temperature in the reaction flask at around -10°C. Stir at this temperature for about 20 minutes and start adding 1.75g (250.0mmol) of lithium metal. The lithium metal should be added in batches, adding about 2 grains each time, specification ∮6mm×10mm, and the time required for adding metal lithium is about 3 to 4 hours. After adding the metal lithium, the temperature is gradually increased to 0°C, and the temperature-maintaining reaction is 9 hours. After the reaction was completed, the excess metal lithium was filtered off, 3.87 g of water was carefully added, tetrahydrofuran and tert-butanol were removed by concentration, 89 g of water was added, and the target product was crystallized to obtain 8.5 g, with a yield of 91%.
References:
CN113620760,2021,A Location in patent:Paragraph 0068-0071
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