Acetaldehyde precursor
A vinyl and ethoxyethoxy technology, which can be used in the preparation of protein-containing food ingredients, organic chemistry, alcoholic beverages, etc., and can solve problems such as changing the characteristics of seasonings
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[0029] Also provided herein is a process for the preparation of spray-dried granules comprising: a) preparing a spray-dried feed emulsion comprising an emulsifier, maltodextrin, and 5-(2-(1-(ethoxyethoxy)propane-2 -yl)-2-methyl-2-vinyltetrahydrofuran or one of its pharmacologically acceptable salts, wherein the emulsion has a buffer adjusted to between 6 and 9. The emulsifier can be selected from gum arabic, saponin And modified starch. Emulsion also can contain optional composition. It can especially also comprise effective amount fireproofing agent or antiknock agent. The type and concentration of this agent in spray-dried emulsion are known to those skilled in the art. As Non-limiting examples of such fire retardants or explosion suppressants include inorganic salts, C 1 -C 12 Carboxylic acid, C 1 -C 12 Salts of carboxylic acids and mixtures thereof. Special antiknock agents are salicylic acid, acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, ca...
Embodiment 1
[0039] Synthesis of 5-(2-(1-ethoxyethoxy)propan-2-yl)-2-methyl-2-vinyltetrahydrofuran
[0040] A mixture of linalool oxide (CAS# 1365-19-1 ) (59 mmol), diethyl ether (50 mL) and p-toluenesulfonic acid (0.06 mmol) was cooled to 5°C. Ethyl vinyl ether (88 mmol) dissolved in diethyl ether (50 mL) was added dropwise over 30 minutes, and the mixture was stirred at room temperature for 12 hours. 5 g of sodium carbonate was added and the mixture was filtered. The product was concentrated using a rotary evaporator and purified by Kugelrohr distillation (70-80 °C, 40 mTorr) to afford 5.19 g (37% yield) of the product (an equimolar mixture of four diastereoisomers) as a colorless oil.
[0041] 1 H NMR (CDCl 3 ,400MHz):δ1.15-1.31(m,15H),1.63-1.76(m,1H),1.79-1.97(m,3H),3.43-3.61(m,2H),3.82-3.94(m,1H) ,4.94-5.07(m,2H),5.14-5.22(m,1H),5.81-6.00(overlapping dd,1H).
[0042] MS(EI):242(M + ,0),169(2),153(38),111(46),93(27),85(18),81(24),73(100),71(31),45(39),43 (47).
Embodiment 2
[0044] Comparative sample 1: Synthesis of 1-ethoxyethyl acetate
[0045] Diethyl ether (50 mL), glacial acetic acid (10 g, 167 mmol) and pTSA (0.01 g) were combined and the mixture was cooled in an ice bath. Ethyl vinyl ether (18 g, 250 mmol) in 50 mL of diethyl ether was added dropwise over 15 minutes. The mixture was removed from the cold bath and stirred at room temperature for 2 hours. Sodium carbonate (5 g) was added and the mixture was filtered. Ether was removed by fractional distillation at atmospheric pressure. The residue was fractionally distilled to obtain 17.7 g (34-35° C., 19 mbar) of 1-ethoxyethyl acetate (134 mmol, 80% yield).
[0046] 1 H NMR (CDCl 3 ,400MHz):δ1.21(t,J=7.1Hz,3H),1.40(d,J=5.2Hz,3H),2.07(s,3H),3.49-3.77(m,2H),5.93(q, J=5.2Hz,1H).
[0047] MS(EI):132(M + ,0),131(<1),117(3),89(5),87(12),73(55),45(61),43(100).
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