ChemicalBook CAS DataBase List Salmeterol Impurity 9

Salmeterol Impurity 9 synthesis

6synthesis methods

Product Name:Salmeterol Impurity 9
CAS Number:97664-58-9
Molecular formula:C16H27NO
Molecular Weight:249.39

97664-55-6 Synthesis

6-N-Benzylamino-1-(4'-phenylbutoxy)Hexane

97664-55-6
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Yield:97664-58-9 97.9%

Reaction Conditions:

with hydrogen;5%-palladium/activated carbon in ethanol at 20; under 760.051 Torr;

Steps:

4 EXAMPLE 4. 6-(4-Phenylbutoxy)hexylamine

A solution of 4.02 g (11.86 mmol) N-benzyl-6-(4-phenylbutoxy)hexylamine in 40 ml EtOH is hydrogenated at room temperature and atmospheric pressure with 0.4 g 5% Pd/C. When 300 ml H2 have been absorbed, the mixture is filtered on decalite and the filtrate is concentrated to yield 2.89 g (97.9%) 6-(4-phenylbutoxy)hexylamine as an oil. RMN 1H (CDCl3), δ (ppm): 1.2-1.8 (m, 12H), 2.65 (c, 4H, -CH2-C6H5+-CH2NH2), 3.4(c, 4H, -CH2-O-CH2-)7.1-7.4(m, 5H, -C6H5).

References:

US6388134,2002,B1 Location in patent:Page column 9