3'-CHLORO-2,2-DIMETHYLPROPIOPHENONE synthesis
- Product Name:3'-CHLORO-2,2-DIMETHYLPROPIOPHENONE
- CAS Number:53226-55-4
- Molecular formula:C11H13ClO
- Molecular Weight:196.67
766-84-7
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$9.00/10g
677-22-5
285 suppliers
$45.00/10ml
53226-55-4
10 suppliers
$417.00/1g
Yield:53226-55-4 87%
Reaction Conditions:
Stage #1: 3-chloro-benzonitrile;tert-butylmagnesium chloride;copper(l) chloride in tetrahydrofuran; for 20 h;Heating / reflux;
Stage #2: with hydrogenchloride in tetrahydrofuran;water at 20;
Stage #3: with water;hydrogenchloride at 90; for 1 h;
Steps:
5C.a
Preparation of N-[4-chloro-2-(2,2-dimethylpropionyl)phenyl]trifluoromethanesulfonamide (Formula 29C). a) To a stirred solution of 3-chlorobenzonitrile (2.0g, 14.54 mmol) and tert-butylmagnesium chloride (1M in THF) (15.99 mL, 15.99 mmol) in THF (10 mL) was added CuCl (29 mg, 0.29 mmol), and the mixture was refluxed for 20 hours. After cooling to RT, cold 1N HCl (10 mL) was added cautiously, the THF removed under reduced pressure, further 1N HCl (20 mL) added and the reaction heated at 90° C. for 1 hour. To the cooled reaction mixture was added water (20 mL) and CH2Cl2 (50 mL), the phases separated, and the aqueous phase again extracted with CH2Cl2. The combined organics were washed with water, dried over MgSO4 and the solvent evaporated under vacuum to afford 1-(3-chlorophenyl)2,2-dimethylpropan-1-one 26C (2.50 g, 87%), as a brown oil.
References:
US2006/63841,2006,A1 Location in patent:Page/Page column 33-34; 8/12
108-37-2
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3282-30-2
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53226-55-4
10 suppliers
$417.00/1g
3282-30-2
370 suppliers
$19.85/100ml
24344-58-9
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53226-55-4
10 suppliers
$417.00/1g
