Laurocapram synthesis
- Product Name:Laurocapram
- CAS Number:59227-89-3
- Molecular formula:C18H35NO
- Molecular Weight:281.48
105-60-2
143-15-7
59227-89-3
Example 1: To a 1 liter reactor were sequentially added 34 g (0.3 mol) of caprolactam, 112 g (0.45 mol) of dodecyl bromide, 300 g of toluene, 3.4 g (3.3 mol %, based on caprolactam) of crystalline tetrabutylammonium hydrogensulphate (TBAHS), and 90 g (2.25 mol) of flaked sodium hydroxide. The resulting non-homogeneous mixture was stirred and reacted at 50°C for 10 hours. Upon completion of the reaction, the mixture was cooled to 40 °C, followed by addition of 135 g of water and continued stirring at the same temperature for 30 min. After the reaction solution was layered, the oil layer was separated and purified by distillation, and the fractions with boiling points ranging from 195°C to 200°C/3mmHg were collected to give 84.0 g of 1-dodecyl azepan-2-one (99.6% yield, based on caprolactam), with a by-production of 0.8 g of dodecyl ether (1.0% yield, based on bromododecane).
105-60-2
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143-15-7
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59227-89-3
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Yield:59227-89-3 99.6%
Reaction Conditions:
with sodium hydroxide in water;toluene;
Steps:
1 EXAMPLE 1
EXAMPLE 1 A 1l reactor is charged with 34 g (0.3 mole) of azacycloheptane-2-one, 112 g (0.45 mole) of dodecyl bromide, 300 g of toluene, 3.4 g (3.3 mole % based on the azacycloheptane-2-one) of crystalline tetrabutylammonium hydrogensulfate (TBAHS) and 90 g (2.25 moles) of flaky sodium hydroxide. This heterogeneous mixture was stirred at 50° C. for 10 hours. After the mixture was cooled to 40° C., 135 g of water was added to the mixture, followed by stirring at 40° C. for 30 minutes. The oil layer was separated and the oil layer thus obtained was subjected to distillation, giving 84.0 g of 1-dodecylazacycloheptane-2-one having a boiling point of 195° to 200° C./3 mmHg (yield of 99.6% based on the azacycloheptane-2-one), and also 0.8 g of dodecyl ether (yield of 1.0% based on the dodecyl bromide).
References:
US4812566,1989,A
143-15-7
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59227-89-3
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112-52-7
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59227-89-3
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105-60-2
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1634-04-4
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143-15-7
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59227-89-3
482 suppliers
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112-53-8
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59227-89-3
482 suppliers
$6.00/25g