1-(1 1-DIMETHYLHEPTYL)-3 5-DIMETHOXYBEN& synthesis
- Product Name:1-(1 1-DIMETHYLHEPTYL)-3 5-DIMETHOXYBEN&
- CAS Number:60526-81-0
- Molecular formula:C17H28O2
- Molecular Weight:264.4
60526-75-2
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60526-81-0
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Yield: 87%
Reaction Conditions:
Stage #1: with ammonia;lithium at -70 - -50;
Stage #2:4-(1',1'-dimethylheptyl)-2,6-dimethoxyphenyl diethylphosphate in tetrahydrofuran;dipentyl ether at -70; for 3 h;
Steps:
2.8
A 1 liter reactor previously cooled at -70° C. was charged with 375 ml of liquid ammonia. Then at a temperature under -50° C., 6.25 g of lithium metal were added. Then, the obtained blue suspension was cooled to -70° C. and during 2 hr a previously prepared solution of 124 g of product (10) (0.3 mole) in 50 ml THF and 250 ml of butyl methyl ether were added. After the addition, the reaction mixture was stirred for an additional hour. At the end of the reaction 25 g of ammonium chloride were carefully added portion wise. The temperature of the resulting light brown solution was slowly increased up to 20° C. Then 375 ml of water were added, which led to ammonia evolution. The reaction mixture was heated up to 85° C. under atmospheric pressure to eliminate ammonia and part of THF/MTBE. Then the reaction mixture was cooled down to room temperature and 375 ml of water and 500 ml of toluene were added. The aqueous phase was then discharged and the toluene phase was washed with 250 ml of water, and again the aqueous phase was discharged. The reaction mixture was then heated up to reflux to remove under atmospheric pressure water and part of the toluene to obtain a 224.5 g of a toluene solution containing about 31% of the product (11) (0.262 mole), about 87% yield.
References:
Aviv, Haim;Bar, Raphael;Schickler, Michael;Amselem, Shimon US2004/110827, 2004, A1 Location in patent:Page/Page column 11
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56469-10-4
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77-78-1
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60526-81-0
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39192-51-3
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60526-81-0
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![Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-](/CAS/20210305/GIF/1000210-73-0.gif)
1000210-73-0
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60526-81-0
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