Indeno[2,1-a]indene-5,10-dione, 4b,9b-dihydro-, (4bS-cis)- (9CI) synthesis
- Product Name:Indeno[2,1-a]indene-5,10-dione, 4b,9b-dihydro-, (4bS-cis)- (9CI)
- CAS Number:74431-35-9
- Molecular formula:C16H10O2
- Molecular Weight:234.25
7584-72-7
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Yield:74431-35-9 86%
Reaction Conditions:
in water at 80 - 150; for 25 h;
Steps:
Synthesis of Intermediate I-2
5.41 g (20 mmol) of Intermediate I-1 was added into 500 ml of polyphosphoric acid (PPA) heated to about 100° C., and was then stirred at about 125° C. for about 21 hours, followed by heating the reaction solution at about 150° C. for a further 2 hours. After the reaction solution was cooled down to about 80° C., 600 ml of water was added thereto, and was then stirred for about 2 hours until a precipitate was obtained. The precipitate was then filtered. The precipitate was dissolved in 140 ml of a hot NaHCO3 aqueous solution, and then stirred for about 30 minutes. The resulting precipitate was filtered, dried for about 12 hours under vacuum conditions to obtain 4.03 g of Intermediate I-2 with a yield of about 86%. This compound was identified using MS/FAB. C16H10O2: calc. 234.25. found 234.38
References:
US2014/27721,2014,A1 Location in patent:Paragraph 0127; 0129
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