Des(oxopentyl) Valsartan Benzyl Ester synthesis
- Product Name:Des(oxopentyl) Valsartan Benzyl Ester
- CAS Number:676129-93-4
- Molecular formula:C26H27N5O2
- Molecular Weight:441.52
![L-Valine, N-[[2'-[1-[(4-methoxyphenyl)methyl]-1H-tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-, phenylmethyl ester](/CAS/20210305/GIF/1307853-55-9.gif)
1307853-55-9
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676129-93-4
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Yield:676129-93-4 84%
Reaction Conditions:
with trifluoroacetic acid in methoxybenzene at 60; for 2.5 h;Inert atmosphere;
Steps:
21.2
Step 2 Under an argon atmosphere, into a 50 ml flask were charged compound 11a (393 mg, 0.7 mmol), trifluoroacetic acid (5.6 mL) and anisole (0.28 mL), and the mixture was stirred at 60° C. for 2.5 hr. The disappearance of the starting material was confirmed TLC (eluent: methanol /chloroform =1/19).After completion of the reaction, the reaction mixture was concentrated, the residue was dissolved in 5% aqueous sodium bicarbonate (50 mL), and the solution was washed with hexane (20 mL ×2). The aqueous layer was adjusted to pH 4.3 with 1N hydrochloric acid, and the precipitated white viscous solid was extracted with ethyl acetate (20 mL ×3). The organic layers were combined, washed with 10% brine (20 mL), dried over magnesium sulfate, and concentrated to compound 12a (261 mg, yield 84%) as a white solid.1H-NMR (400 MHz, CDCl3) δ=0.90 (3H, d, J=6.4), 0.95 (3H, d, J=6.8), 2.13-2.28 (1H, m), 3.49 (1H, d, J=4.4), 3.77-3.90 (2H, m), 5.19 (2H, dd, J=12.0, 29.2), 6.75-7.10 (4H, m), 7.27-7.56 (9H, m).IR(KBr) ν(cm-1):1742, 1668, 1604 EIMS (m/z):441(M+) melting point: 53.5-57.2° C.
References:
US2012/232283,2012,A1 Location in patent:Page/Page column 34-35
18039-42-4
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676129-93-4
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98-88-4
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676129-93-4
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21388-92-1
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676129-93-4
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873-75-6
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676129-93-4
16 suppliers
$139.80/10mg