Methyl isobutyrylacetate synthesis
- Product Name:Methyl isobutyrylacetate
- CAS Number:42558-54-3
- Molecular formula:C7H12O3
- Molecular Weight:144.17
563-80-4
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Yield:42558-54-3 88%
Reaction Conditions:
Stage #1: 3-methyl-butan-2-onewith sodium hydride in 1,4-dioxane;mineral oil at 20; for 0.166667 h;
Stage #2: carbonic acid dimethyl ester in 1,4-dioxane;mineral oil at 50; for 3 h;Reagent/catalyst;Solvent;Temperature;Time;
Steps:
Preparation of Methyl 4-Methyl-3-oxopentanoate[4b] (2)
Methyl isopropyl ketone (10.00 g,116.10 mmol) was added slowly to a suspension of sodium hydride (60 % in mineral oil, 9.29 g, 232.25 mmol) in 1,4-dioxane (70 mL). The mixture was stirred at room temperature for 10 min. Dimethyl carbonate (15.70 g, 174.31 mmol) was added and the mixture was stirred at 50 °C for 3 h. The mixture was cooled to room temperature, and acetic acid (14mL) was slowly added. The precipitate was filtered and washed with 1,4-dioxane(20 mL). The filtrate was concentrated unde rvacuum. Compound 2 was collected at 80-85 °C under vacuum (～10 mbar)as colorlessl iquid (14.73g, yield 88 %). 1H NMR (600 MHz,CDCl3) δ: 3.69 (s,3H), 3.48 (s,2H), 2.68 (m,1H), 1.01 (d, J7.2 Hz, 6H). 13C NMR (150 MHz,CDCl3) δ: 205.95, 167.38, 51.44, 46.23, 40.44, 17.26.
References:
Xing, Yuzhi;Chen, Shipeng;Zhou, Yingtao;Liu, Na;Chen, Ligong;Li, Yang [Synthetic Communications,2015,vol. 45,# 24,p. 2832 - 2840]
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