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Acetic Acid → 2-{[3-(2,3,4-tri-O-benzyl-alpha-L-fucopyranosyl)propyl]amino}ethyl 2-(acetylamino)-2-deoxy-beta-D-glucopyranoside

HRID 1488288
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1488288
[CH2:1]([O:8][C@H:9]1[C@H:14]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C@H:13]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C@H:12]([CH3:31])[O:11][C@H:10]1[CH2:32][CH2:33][CH:34]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O:39][C@H:40]1[C@H:49]([O:50]C(=O)C)[C@@H:48]([CH2:54][O:55]C(=O)C)[O:47][C@@H:42]([O:43][CH2:44][CH2:45][NH2:46])[C@@H:41]1[NH:59][C:60](=[O:62])[CH3:61])(=O)C.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].O(C)[Na]>C(Cl)Cl.CO>[C:60]([NH:59][C@@H:41]1[C@@H:40]([OH:39])[C@H:49]([OH:50])[C@@H:48]([CH2:54][OH:55])[O:47][C@H:42]1[O:43][CH2:44][CH2:45][NH:46][CH2:34][CH2:33][CH2:32][C@@H:10]1[O:11][C@@H:12]([CH3:31])[C@@H:13]([O:23][CH2:24][C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[C@@H:14]([O:15][CH2:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[C@@H:9]1[O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)(=[O:62])[CH3:61]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 176Acetic AcidHCID 5049666Sodium triacetoxyborohydrideHCID 152815833-(2,3,4-tri-O-benzyl-alpha-L-fucopyranosyl)propanalHCID 542114332-aminoethyl 3,4,6-tri-O-acetyl-2-(acetylamino)-2-deoxy-beta-D-glucopyranosideHCID 178418582HCID 178418582, Verbindung

Produkt 1

HCID 118005652
2-{[3-(2,3,4-tri-O-benzyl-alpha-L-fucopyranosyl)propyl]amino}ethyl 2-(acetylamino)-2-deoxy-beta-D-glucopyranoside

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a mixture of 3-(2,3,4-tri-O-benzyl-α-L-fucopyranosyl)propanal (800 mg, 1.69 mmol) and 2-aminoethyl 3,4,6-tri-O-acetyl-2-(acetylamino)-2-deoxy-β-D-glucopyranoside (987 mg, 2.53 mmol) in CH2Cl2 (15 mL) was added acetic acid (29 μL, 0.506 mmol) and sodium triacetoxyborohydride (893 mg, 4.21 mmol). After stirring at rt overnight, the reaction mixture was concentrated and the residue was taken up in EtOAc (70 mL), washed with sat'd NaHCO3 (2×100 mL), brine (30 mL), dried over Na2SO4, filtered and concentrated. The residue was taken up in CH3OH (8 mL), to which NaOCH3 (27 mg, 0.506 mmol) was added. After stirring at rt for 2 hr, the resulting mixture was concentrated and the residue was purified by flash chromatography on C18 reverse phase silica gel (120 g), eluting with 5-100% AcCN in water to give the title compound. 1H NMR (CDCl3, 400 MHz) δ 1.30 (d, J=6.6, 3H), 1.50 (m, 1H), 1.60 (m, 1H), 1.68 (m, 1H), 2.02 (s, 3H), 2.64 (m, 2H), 2.81 (m, 2H), 3.39 (m, 1H), 3.57 (m, 2H), 3.69 (m, 1H), 3.78-3.85 (m, 4H), 3.92 (m, 2H), 4.00 (m, 2H), 4.45 (d, J=7.7, 1H), 4.52 (d, J=11.9, 1H), 4.62 (d, J=11.8, 1H), 4.68 (d, J=12.1, 1H), 4.79 (d, J=12.0, 2H), 7.28-7.38 (m, 15H), 7.65 (s, 1H); [M+H/e]+=723.3925.

Aufarbeitung

  1. concentrationthe reaction mixture was concentrated
  2. washwashed with sat'd NaHCO3 (2×100 mL), brine (30 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. additionwas added
  7. stirringAfter stirring at rt for 2 hr
  8. concentrationthe resulting mixture was concentrated
  9. customthe residue was purified by flash chromatography on C18 reverse phase silica gel (120 g)
  10. washeluting with 5-100% AcCN in water

Quellen und Nachweise

ORD-Eintrag
ord-a5a572e76bc743f19bd50a147cdea512
Quelldatensatz
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09427475B2

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