3,5-Diacetoxyacetophenone synthesis
- Product Name:3,5-Diacetoxyacetophenone
- CAS Number:35086-59-0
- Molecular formula:C12H12O5
- Molecular Weight:236.22
Yield:35086-59-0 87%
Reaction Conditions:
tris(dibenzoylmethane)iron in tetrahydrofuran at -15; for 0.5 h;Product distribution / selectivity;Inert atmosphere;Grignard Reaction;
Steps:
4.3
Under a nitrogen atmosphere a 100 ml three-necked flask with magnetic stirrer, thermometer, dropping funnel and condenser was charged with 2 g (7.8 mmol) of diacetoxybenzoyl chloride, 169 mg (3mol-% based on acid chloride) of tris(dibenzoylmethanato) iron and 15 ml of dry THF. 2.6 ml of methylmagnesium chloride (3M in THF) were added dropwise to the solution over a period of 20 minutes. The reaction mixture was kept under stirring for further 10 minutes at -15 °C. The mixture was then quenched with aqueous ammonium chloride. After extraction of the mixture with ethyl acetate the extract was dried over MgSO4 and concentrated. The residue was analyzed by GC. The yield was 87.0 %.
References:
DSM IP Assets B.V. EP2404891, 2012, A1 Location in patent:Page/Page column 5
51863-60-6
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