3-4-dimethylpropiophenone synthesis
- Product Name:3-4-dimethylpropiophenone
- CAS Number:17283-12-4
- Molecular formula:C11H14O
- Molecular Weight:162.23
104174-13-2
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17283-12-4
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Yield:-
Reaction Conditions:
with pyridinium chlorochromate in dichloromethane; for 0.75 h;Silica gel;
Steps:
1.6
Step 6: To a mixture of 3,4-dimethylbenzaldehyde (1 i; 500 mg, 3.73 mmol) and Et2O (12 mL) is added ethylmagnesium bromide (3M, 1.4 mL, 1.2 mmol) dropwise. After 15 min, the reaction is quenched with saturated aqueous NH4CI (50 mL) and the layers are separated. The organic layer is washed with saturated aqueous NH4CI (50 mL), dried over Na2SO4 and concentrated to give the intermediate benzyl alcohol. To a mixture of this material and DCM (28 mL) is added silica gel (2.2 g) followed by pyridinium chlorochromate (1.5 g, 7.2 mmol). The mixture is stirred for 45 min and the mixture is filtered through a plug of silica (3 x 1.5 cm) which is then washed with DCM (total of 50 mL). The filtrate is evaporated to dryness to give the intermediate ketone. This material is combined with sodium acetate (102 mg, 1.25 mmol) and hydroxylamine hydrochloride (87 mg, 1.25 mmol) in MeOH (0.8 ml.) and is heated to 85°C in a sealed tube. After 1 h, the reaction is allowed to cool to room temperature and concentrated onto silica gel (2 g). The product is purified by CombiFlash Companion to give the oxime 1j as a mixture of cis- and trans- isomers.
References:
WO2010/130034,2010,A1 Location in patent:Page/Page column 42; 43-44
95-47-6
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5973-71-7
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17283-12-4
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123-62-6
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17283-12-4
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