1H-Inden-1-one, 2-acetyl-5-fluoro-2,3-dihydro- synthesis
- Product Name:1H-Inden-1-one, 2-acetyl-5-fluoro-2,3-dihydro-
- CAS Number:1263382-10-0
- Molecular formula:C11H9FO2
- Molecular Weight:192.19
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Yield:-
Reaction Conditions:
Stage #1: 5-fluoro-1-indanone;ethyl acetatewith sodium hydride in tetrahydrofuran;mineral oil at 30 - 50; for 3.25 h;Inert atmosphere;
Stage #2: with hydrogenchloride in tetrahydrofuran;water;mineral oil at 30; pH=~ 5;
Steps:
2
Into a 250 mL round bottom flask equipped with nitrogen gas flow are placed sodium hydride (1 .6 g, 60% dispersion in mineral oil), THF (15 mL), 5- fluoro-1 -indanone (3 g), and ethyl acetate (3.52 g), and the mixture is stirred at 30°C for about 15 minutes. The mixture is heated to 50°C and maintained for about 3 hours under a nitrogen atmosphere. After reaction completion, the mixture is cooled to 300C, ice water (40 mL) is added, and pH is adjusted to about 5 using 10% aqueous HCI (4 mL). The mixture is extracted with ethyl acetate (90 mL) and the organic layer is concentrated under reduced pressure below 55°C.lsopropanol (15 mL) is added to the residue and stirred for about 1 hour at 30°C. The solid is filtered and washed with isopropanol (15 ml_), to obtain 2.3 g of the title compound as a solid.1HNMR (CDCI3, 400 MHz): 2.16(s, 3H), 3.52(s, 2H), 7.0-7.89(3H, m, ArH), 14.52-14.90 (S1 CH-OH).Mass: M+1 (M.Wt.: 193).
References:
WO2011/14613,2011,A2 Location in patent:Page/Page column 11; 12
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