Ethyl isovalerate synthesis
- Product Name:Ethyl isovalerate
- CAS Number:108-64-5
- Molecular formula:C7H14O2
- Molecular Weight:130.18
638-10-8
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108-64-5
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Yield:108-64-5 99%
Reaction Conditions:
with C40H56FeN2Si4(2-);hydrogen in 1,2-dimethoxyethane at 80; under 7600.51 Torr; for 2 h;Schlenk technique;Autoclave;
Steps:
17 [Example 17] Hydrogenation of ethyl 2,3-dimethylacrylate
A 20-mL Schlenk tube equipped with a magnetic stirrer was heat dried while pumping to a vacuum of 5 Pa before its interior was purged with argon atmosphere. Into the Schlenk tube, iron complex A (7.3 mg, 0.01 mmol) was admitted as catalyst and dissolved in dimethoxyethane (2 mL). To the solution, ethyl 2,3-dimethylacrylate (128 mg, 1.0 mmol) was added. The solution was transferred into an autoclave, whose interior was purged with hydrogen. In a hydrogen atmosphere of 10 atm., the solution was stirred at 80° C. for 2 hours. With anisole (108 mg, 1.0 mmol) added as internal standard, the geometry and yield of the product were determined by 1H-NMR spectroscopy. The resulting compound was identified for geometry by 1H and 13C-NMR spectroscopy. The results are shown as Entry 5 in Table 4. H-NMR (CDCl3, 400 MHz) δ=0.93-0.96 (m, 6H, Me), 1.28 (t, 3H, OCH2CH3), 2.00-2.04 (m, 1H, CH and CH2C(═O)), 4.19 (q, 2H, OCH2CH3) C-NMR (CDCl3, 100 MHz) δ=14.6, 22.9, 26.0, 43.6, 60.3, 173.5
References:
US10363551,2019,B2 Location in patent:Page/Page column 31; 34
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