Diethyl Methyl-D3-malonate synthesis
- Product Name:Diethyl Methyl-D3-malonate
- CAS Number:54840-57-2
- Molecular formula:C8H11D3O4
- Molecular Weight:0
Yield:54840-57-2 87%
Reaction Conditions:
Stage #1: diethyl malonatewith sodium in ethanol at 0; for 0.5 h;
Stage #2: iodomethane-d3 in ethanol at 0 - 20; for 5 h;
Steps:
3.1
Step l[00140] d3-diethyl 2-methylmalonate: sodium metal (7.59 g, 330.00 mmol, 1.05 equiv.) was slowly added to ethanol (500 mL) and stirred at ambient temperature until all the sodium metal was consumed. At about 0 0C, diethyl malonate (50 g, 312.50 mmol, 1.00 equiv.) was added dropwise, over a period of 30 minutes, to the stirred solution. At about 0 0C, iodomethane-6?3 (47.85 g, 330.00 mmol, 1.05 equiv) was then added dropwise, over a period of about 2 hours, to the stirred solution. The solution was stirred at ambient temperature for about 3 hours and then concentrated in vacuo. After adding water (500 mL), standard extractive workup with ethyl acetate (3 x 300 mL) afforded the title product as a light yellow liquid (48 g; yield = 87 %). 1H NMR (300 MHz, CDCl3) δ: 4.15 (q, J = 7.2 Hz, 2 H), 2.30 (s, I H), 1.28 (X, J = 7.2 Hz, 3 H).
References:
WO2011/17108,2011,A2 Location in patent:Page/Page column 52
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