ChemicalBook CAS DataBase List 2-(1-Cyclohexenyl)ethylamine

2-(1-Cyclohexenyl)ethylamine synthesis

8synthesis methods

Product Name:2-(1-Cyclohexenyl)ethylamine
CAS Number:3399-73-3
Molecular formula:C8H15N
Molecular Weight:125.21

125 ml of ethylamine was placed in a 250 ml three-necked flask, which had previously been flushed with argon, at -70 ° C. 6.27 g (50 mmol) of 2-phenylethylamine was added. The resulting clear, colorless solution was metered in with 1.14 g (164.2 mmol) of Li powder; the solution turned dark blue 5 minutes after the onset of turbidity. After stirring for 2 hours at -70 ° C, the mixture was warmed to -30 ° C. Then another 0.24 g (34.6 mmol) of Li powder was added. After stirring again at -30 ° C. for 2 hours, the cooling bath was removed. The reaction mixture was allowed to warm to room temperature overnight. The reaction mixture was then given 25 ml of abs. After that, a gray suspension formed. After stirring for 20 minutes at room temperature, 25 ml of water was slowly added (exothermic temperature 40 ° C.). The excess ethylamine was then distilled off at 40 °C. The distillation residue was evaporated to dryness. Then, 100 ml of water was added and extracted 3 times with 80 ml chloroform. The combined organic phases were dried over Na?SO?, filtered, and evaporated. The 2-(1-Cyclohexenyl)ethylamine was obtained in a GC yield of 69.8%.

6975-71-9 Synthesis

6975-71-9
157 suppliers
$25.00/5g

3399-73-3
271 suppliers
$13.00/5g

Yield:3399-73-3 95%

Reaction Conditions:

with sodium bis(2-methoxyethoxy)aluminium dihydride in tetrahydrofuran at 15; for 21 h;Inert atmosphere;Green chemistry;Solvent;

Steps:

1.1; 1.2; 2.1; 2.2 Example 2:
11-cyclohexenyl ethylamine crude preparations: Under argon protection,121 g of 1-cyclohexene acetonitrile (1.0 mol 1.0 eq) was added to the reaction flask.Tetrahydrofuran 1000mL,577.6 g (2 mol 2.0 eq 70%) of red aluminum solution was slowly added dropwise at 15±5 degrees.After about 1 hour, the reaction was stirred at this temperature for 20 hours;The mixture was slowly added dropwise to 1500 mL of (10% NaOH) aqueous solution to quench the reaction, and filtered.The mother liquor was layered, and the aqueous phase was extracted twice with diethyl ether 500 mL, and the organic phases were combined.The organic layer was dried over sodium2Preparation of pure 1-cyclohexeneethylamine:To the reaction flask, 130 g of crude 1-cyclohexeneethylamine was added, and the pressure was reduced to 5-10 mmHg, and distilled at 70-120 °C to obtain 119 g of a pure 1-cyclohexeneethylamine, 95%.

References:

Liaoning Dong Ke Pharmaceutical Co., Ltd.;Cong Qiang;Li Wan;Mao Chunfeng;Hu Yushan;Liu Sihan CN108821978, 2018, A Location in patent:Paragraph 0037-0042

FullText

6975-71-9 Synthesis

6975-71-9
157 suppliers
$25.00/5g

4442-85-7 Synthesis