1,2-Dichloroethane → HCID 86624523, Verbindung

HRID 269689Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 269689
[CH2:1]([O:8][C:9]([NH:11][CH2:12][C@@H:13]([C:22]([OH:24])=O)[NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1(NC2CCCCC2)CCCCC1.[C:38]([O:42][C:43](=[O:48])[NH:44][CH2:45][CH2:46][NH2:47])([CH3:41])([CH3:40])[CH3:39].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C)C=O.C(N(CC)CC)C>[CH2:1]([O:8][C:9](=[O:10])[NH:11][CH2:12][C@H:13]([NH:14][C:15]([O:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[O:16])[C:22]([NH:47][CH2:46][CH2:45][NH:44][C:43]([O:42][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:48])=[O:24])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

7

Edukt 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 187201N-BOC-ethylenediamineHCID 2755949Boc-Dap(Z)-OH.DCHA

Produkt 1

HCID 86624523HCID 86624523, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

Under argon, 0.50 g (0.96 mmol) of 3-{[(benzyloxy)carbonyl]amino}-N-(tert-butoxycarbonyl)-L-alanine-N-cyclohexylcyclohexanamine (1:1) and 0.154 g (0.96 mmol) of tert-butyl(2-aminoethyl)carbamate are dissolved in 10 ml of dimethylformamide and 0.5 ml of triethylamine. Then, at 0° C. (ice bath), 0.314 g (1.64 mmol) of EDC and 0.043 g (0.32 mmol) of HOBt are added. The mixture is slowly warmed to RT and stirred at RT for 12 h. The solution is concentrated in vacuo and the residue is taken up with ethyl acetate. The organic phase is washed successively with saturated sodium bicarbonate and sodium chloride solutions, dried over magnesium sulfate and evaporated in vacuo. The remaining solid is dried to constant weight under high vacuum.

Aufarbeitung

  1. concentrationThe solution is concentrated in vacuo
  2. washThe organic phase is washed successively with saturated sodium bicarbonate and sodium chloride solutions
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe remaining solid is dried to constant weight under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-5c1defd9cec04710b811109e08c11e87
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07446102B2

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