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CAS No. : | 16937-91-0 | MDL No. : | MFCD00063115 |
Formula : | C13H18N2O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | VULSXQYFUHKBAN-LLVKDONJSA-N |
M.W : | 266.29 | Pubchem ID : | 7272528 |
Synonyms : |
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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: |
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* 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 |
---|---|---|
With thionyl chloride; In methanol; at 0 - 20℃; for 18h;Inert atmosphere; | Boc-D-Orn(Cbz)-OH (400 mg, 1.09 mmol, 1.00 equiv) was dissolved in CH3OH (2.30 mL) at0 C. Then, freshly distilled thionylchloride (773 mg, 6.50 mmol, 5.95 equiv) was added dropwise. The reaction mixture was stirred at 0 C rt. After 18 h, the solvent was removed under reduced pressure. The resulting residue was charged with Et2O and the solvent was removed under reduced pressure. This procedure was repeated several times. The crudeproduct 22 was used without further purification. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With chloro-trimethyl-silane; N-ethyl-N,N-diisopropylamine; In dichloromethane; | Example 74A N5-[Benzyloxycarbonyl]-N2-[(9H-fluoren-9-ylmethoxy)carbonyl]-D-ornithine N5-[(Benzyloxy)carbonyl]-D-ornithine (3.8 g, 14.27 mmol) [Ulhaq, Saraj et al.; Bioorg. Med. Chem.; EN; 7; 9; 1999; 1787-1796] is provided in dichloromethane (190 ml), DIEA (2.4 ml, 1.8 g, 17.27 mmol, 1 eq.) and chlorotrimethylsilane (3.6 ml, 3.1 g, 28.53 mmol, 2 eq.) are added, and the mixture is stirred under reflux overnight. The reaction is cooled (0 C.) and DIEA (4.7 ml, 3.7 g, 28.54 mmol, 2 eq.) again and (9-fluorenylmethyl) chloroformate (3.7 g, 14.27 mmol, 1 eq.) are added, and the mixture is warmed to RT and stirred at this temperature overnight. For the workup, the reaction is diluted with dichloromethane and washed with a 10% aq. citric acid solution, the organic phase is dried over sodium sulfate, the solvent is removed on a rotary evaporator and the mixture is dried in vacuo. 6.5 g (93.2% of theory) of the title compound are obtained. LC-MS (Method 18): Rt=2.57 min; MS (ESIpos): m/z (%)=489 (100) [M+H]+, 977 (100) [2M+H]+; MS (ESIneg.): m/z (%)=487 (80) [M-H]-, 975 (100) [2M-H]-. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92% | Compound 5 (22 g, 82.6 mmol) was dissolved/suspended in an aqueous solution (250 mL) of potassium carbonate (12.56 g, 90.9 mmol) and 1,4-dioxane (100 mL) was added. Di-tert-butyl dicarbonate (18.93 g, 86.75 mmol) was added dropwise in 1,4-dioxane (200 mL) over a period of 60 min. The mixture was stirred at rt overnight, then concentrated under reduced pressure to a volume of about 150 mL. Water (50 mL) was added and the pH was adjusted to 2-3 by the addition of 1 M aq hydrochloric acid (about 150 mL). The product was extracted with ethyl acetate (400 mL and 3 × 300 mL) and the combined organic phases were treated with 10 mM aq hydrochloric acid (100 mL), saturated aq NH4Cl (200 mL), water (100 mL) as well as brine (250 mL) prior to drying over sodium sulfate. Filtration and evaporation of the solvent yielded a yellowish oil which turned into a foam that hardened to a solid during drying in vacuo (27.8 g, 92%). 1H NMR (300 MHz, DMSO-d6): delta (ppm) 1.38 (s, 9H), 1.4-1.59 (m, 3H), 1.65 (m, 1H), 2.98 (m, 2H), 3.83 (m, 1H), 5.0 (s, 2H), 7.07 (d, 1H, 3J = 8.0 Hz), 7.25 (t, 1H, 3J = 5.5 Hz), 7.34 (m, 5H), 12.42 (s, 1H); C18H28N2O6 (366.4). |
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