4,4'-Dihydroxybenzophenone synthesis
- Product Name:4,4'-Dihydroxybenzophenone
- CAS Number:611-99-4
- Molecular formula:C13H10O3
- Molecular Weight:214.22
90-96-0
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611-99-4
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Yield:611-99-4 89%
Reaction Conditions:
with potassium carbonate;3-mercaptopropionic acid in ISOPROPYLAMIDE at 150; for 18 h;
Steps:
5
Example 5: Preparation of 4,4'-dihydroxybenzophenone.A mixture of 4,4'-dimethoxybenzophenone (1.21 g, 5.0 mmol), potassium carbonate (8.3 g, 60 mmol), 3-mercaptopropionic acid (4.24 g, 40 mmol) and dimethylacetamide (50 mL) is stirred at 150 °C for 18 h and the solvent is removed under reduced pressure. Water is added (30 mL), followed by 37 % hydrochloric acid (8 mL) and the product is extracted with MTBE (3 * 25 mL) and ethyl acetate (2 * 25 mL). The organic phases are combined, dried with sodium sulfate and concentrated under reduced pressure. The crude is purified by chromatography (silica gel; hexane : ethyl acetate = 50 : 50), crystallized from water and dried under reduced pressure to yield 0.95 g (89 % yield) of 4,4'-dihydroxybenzophenone. 1H NMR (DMSO-d6): δ 6.87 (m, 4H), 7.60 (m, 4H), 10.29 (s, 2H).
References:
LEK PHARMACEUTICALS D.D.;CASAR, Zdenko;FURLAN, Borut WO2011/154152, 2011, A1 Location in patent:Page/Page column 16
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