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CAS No. : | 146844-02-2 | MDL No. : | MFCD00190908 |
Formula : | C19H22ClNO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | GRGJVECUQLAEDM-UNTBIKODSA-N |
M.W : | 363.84 | Pubchem ID : | 45789900 |
Synonyms : |
|
Chemical Name : | (R)-Dibenzyl 2-aminopentanedioate hydrochloride |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62% | With triethylamine; In propan-1-ol; at 0 - 5℃; for 3.0h;Heating / reflux; | Intermediate 1.4; benzyl l-(3-cyclohexyl-3-oxopropyl)-5-oxo-D- prolinate; In a flame-dried, nitrogen- flushed IL round bottom flask with magnetic stirrer, D-Dibenzyl glutamate hydrochloride (H-D-GIu(OBn)-OBn) (0.04mol, 14.6g) was dissolved in anhydrous 1-propanol (0.5L). To the resulting solution cooled by ice bath, triethylamine (0.15mol, 21ml) was added at stirring under nitrogen. The mixture was stirred for 10 min followed by addition of freshly prepared vinylcyclohexylketone (0.05 mol). The reaction mixture was stirred under nitrogen at 0-50C for 3h until reaction was complete (Control by LC-MS and NMR of concentrated aliquots).When the reaction was complete, the cooling was removed, reflux condenser attached to the flask, and the mixture was refluxed overnight in an oil bath. The yellow solution was concentrated, diluted with a mixture of chloroform-hexanes (1:1 v/v, 100ml), and filtered from white needles Of Et3NHCl. The filtrate was concentrated again giving 26.1 g of light yellow oil. Purification on 20Og of silica gel, EPO <DP n="61"/>eluent hexanes-EtOAc from 100:0 to 0:100, gave 8.85g (62percent) of pure benzyl l-(3- cyclohexyl-3-oxopropyl)-5-oxo-D-prolinate as clear oil, Rf 0.30 (hexanes-EtOAc 1:4). 1H NMR (400 MHz, CDCl3 ) delta 7.36 (m, 5H, Ph), 5.19 (d, IH, 12.0Hz, CH2Ph), 5.15 (d, IH, 12.0Hz, OCH2Ph), 4.33 (m, IH, CH-COOBn), 4.11 (m, IH, cyclohexyl CH-CO), 3.62 (m, IH, CH2-N), 3.37 (m, IH, CH2-N), 2.89 (m, IH, chain CH2-CO), 2.66 (m, IH, chain CH2-CO), 2.43 (m, IH, lactam ring CH2-CO), 2.30 (m, IH, lactam ring CH2-CO), 2.27 (m, IH, lactam ring H3) 2.02 (m, IH, lactam ring H3), 1.85-1.55 (m, 5H, cyclohexyl), 1.30-1.15 (m, 5H, cyclohexyl). 13C NMR (100 MHz, CDC13) delta 211.9 (CO-C6Hn), 175.0 (-CO-N), 171.7 (COOBn), 135.0 (ipso-C Ph), 128.5, 128.2 (o-C, m-C Ph), 128.4 (p-C Ph), 67.5 (OCH2-Ph), 61.7 (CH-COOBn), 51.2 (cyclohexyl CH-CO), 39.2 (chain CH2CO), 38.2 (CH2-N), 30.1 (lactam ring CH2-CO), 29.0, 26.5, 26.3 (cyclohexyl), 24.1 (lactam ring C3). |
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