D-Lysine hydrochloride synthesis
- Product Name:D-Lysine hydrochloride
- CAS Number:7274-88-6
- Molecular formula:C6H15ClN2O2
- Molecular Weight:182.65
7274-88-6
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28957-33-7
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$45.00/50mg
Yield:28957-33-7 15%
Reaction Conditions:
with hexamethyldisilazan in toluene; for 168 h;Heating / reflux;
Steps:
2.a
a) 3R-Amino-azepan-2-one D-Lysine hydrochloride (48 g, 0.26 mol) and hexamethyldisilazane (424.4 g, 2.6 mol) were suspended in toluene (1.1 litre) and refluxed for 1 week under an argon atmosphere, using a water-trap condenser. The reaction mixture was cooled to r.t. and slowly added to ice-cold MeOH (2.24 litre). The resultant clear solution was stirred for 30 min and concentrated under reduced pressure. The white, waxy solid was stirred in ethyl acetate, filtered and the filtrated concentrated under reduced pressure: white solid 5.4 g, (15%); 1H NMR (CDCl3) δ 1.35-2.05 (m, 8H), 3.2-3.26 (m, 2H), 3.53 (dd, 1H), 6.10 (br, 1H) MS: m/e=129.2 (MH+)
References:
US2006/14945,2006,A1 Location in patent:Page/Page column 41
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