2'-(DIFLUOROMETHOXY)ACETOPHENONE 98 synthesis
- Product Name:2'-(DIFLUOROMETHOXY)ACETOPHENONE 98
- CAS Number:127842-55-1
- Molecular formula:C9H8F2O2
- Molecular Weight:186.16
65094-22-6
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127842-55-1
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Yield: 92%
Reaction Conditions:
with potassium hydroxide in water;acetonitrile at -20 - 20; for 1.15 h;
Steps:
1- [2-(Difluoromethoxy)phenyllethan- 1-one
Potassium hydroxide (105 g, 1872 mmol) was suspended in a mixture of acetonitrile (200 mL) and water (200 mL) and cooled to approximately -20°C. 1-(2-Hydroxyphenyl)ethanone (11.28 mL, 93.7 mmol) was added dropwise, followed by diethyl [bromo(difluoro)methyl]phosphonate (33.27 mL, 187.3 mmol) over 15 minutes. The mixture was then allowed to warm to room temperature over 1 h. The mixture was extracted with ethyl acetate (3 x 200 mL), then the combined organic layers were washedwith brine (50 mL), dried over magnesium sulfate and concentrated under vacuum. The mixture was purified by flash chromatography to afford the title compound (16.0 g, 92%) as a colourless oil. Method B HPLC-MS: MH+ m/z 187, RT 1.77 minutes.
References:
UCB PHARMA S.A.;BENTLEY, Jonathan Mark;BROOKINGS, Daniel Christopher;BROWN, Julien Alistair;CAIN, Thomas Paul;CHOVATIA, Praful Tulshi;FOLEY, Anne Marie;GALLIMORE, Ellen Olivia;GLEAVE, Laura Jane;HEIFETZ, Alexander;HORSLEY, Helen Tracey;HUTCHINGS, Martin Clive;JACKSON, Victoria Elizabeth;JOHNSON, James Andrew;JOHNSTONE, Craig;KROEPLIEN, Boris;LECOMTE, Fabien Claude;LEIGH, Deborah;LOWE, Martin Alexander;MADDEN, James;PORTER, John Robert;QUINCEY, Joanna Rachel;REED, Laura Claire;REUBERSON, James Thomas;RICHARDSON, Anthony John;RICHARDSON, Sarah Emily;SELBY, Matthew Duncan;SHAW, Michael Alan;ZHU, Zhaoning WO2014/9295, 2014, A1 Location in patent:Page/Page column 112
65094-22-6
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$6.00/1g
118-93-4
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$10.00/25g
![Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-](/CAS/20210305/GIF/1000210-73-0.gif)
1000210-73-0
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127842-55-1
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$18.00/250mg
