1,1-diethoxy-3-phenylacetone synthesis
- Product Name:1,1-diethoxy-3-phenylacetone
- CAS Number:19256-31-6
- Molecular formula:C13H18O3
- Molecular Weight:222.28
6921-34-2
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Yield:19256-31-6 93%
Reaction Conditions:
in tetrahydrofuran at -78; for 12 h;
Steps:
23.1 Step 1: Preparation of 1,1-diethoxy-3-phenylpropane-2-one
5.29 g (30.0 mmol) of ethyl diethoxyacetate was dissolved in anhydrous THF (50 mL), which was frozen at -78° C. PhMgCl (2M THF solution, 1.5 equivalent) was added slowly thereto for 5 minutes, followed by stirring for 12 hours.
While cooling the reaction mixture with ice water, saturated NH4Cl aqueous solution (50 mL) was slowly added thereto.
The reaction mixture was extracted by using ethyl acetate.
The extracted organic layer was washed with saturated brine, separated, dried (Na2SO4), and concentrated under reduced pressure.
The obtained compound was separated by column chromatography (SiO2, eluent:
hexane/ethyl acetate, 20/1->hexane/ethylacetate, 5/1) to give 6.21 g of the target compound 1,1-diethoxy-3-phenylpropane-2-one as a colorless oil (27.9 mmol, yield: 93%).
1H NMR(300 MHz, CDCl3) δ 7.18-7.35 (m, 5H), 4.63 (s, 1H), 3.89 (s, 2H), 3.63-3.71 (m, 2H), 3.47-3.61 (m, 2H), 1.19-1.27 (m, 6H).
References:
US2018/105527,2018,A1 Location in patent:Paragraph 0729-0731
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