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Diisopropylethylamine → Benzyl 4-(1-(2-(benzyloxy)-2-oxoethyl)cyclopentylamino)-2-(biphenyl-4-ylmethyl)-4-oxobutanoate

HRID 333307
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Reaktionsgleichung

Reaktionsgleichung von HRID 333307
Cl.[NH2:2][C:3]1([CH2:8][C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])[CH2:7][CH2:6][CH2:5][CH2:4]1.[CH2:19]([O:26][C:27](=[O:46])[CH:28]([CH2:33][C:34]1[CH:39]=[CH:38][C:37]([C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)=[CH:36][CH:35]=1)[CH2:29][C:30](O)=[O:31])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.CCN=C=NCCCN(C)C.Cl.ON1C2N=CC=CC=2N=N1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH2:12]([O:11][C:9](=[O:10])[CH2:8][C:3]1([NH:2][C:30](=[O:31])[CH2:29][CH:28]([CH2:33][C:34]2[CH:35]=[CH:36][C:37]([C:40]3[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=3)=[CH:38][CH:39]=2)[C:27]([O:26][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:46])[CH2:7][CH2:6][CH2:5][CH2:4]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1
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Komponenten

7

Edukt 5

HCID 81531DiisopropylethylamineHCID 181649HOAtHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 68749504Benzyl 2-(1-aminocyclopentyl)acetate hydrochlorideHCID 687501454-(Benzyloxy)-3-(biphenyl-4-ylmethyl)-4-oxobutanoic acid

Produkt 1

HCID 68751041
Benzyl 4-(1-(2-(benzyloxy)-2-oxoethyl)cyclopentylamino)-2-(biphenyl-4-ylmethyl)-4-oxobutanoate
Ausbeute 75,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of benzyl 2-(1-aminocyclopentyl)acetate hydrochloride (66 mg, 0.245 mmol), 4-(benzyloxy)-3-(biphenyl-4-ylmethyl)-4-oxobutanoic acid (78 mg, 0.209 mmol), WSC.HCl (60.1 mg, 0.314 mmol) and 1-hydroxy-7-azabenzotriazole (42.7 mg, 0.314 mmol) in DMF (2 ml) was added DIPEA (0.055 ml, 0.314 mmol) at room temperature. After stirred for 4 hours, the reaction was quenched with H2O. The product was extracted with EtOAc, and the organic layer was washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The obtained residue was purified by flash column chromatography on silica gel (eluent: heptane/EtOAc=100:0 to 0:100) to give benzyl 4-(1-(2-(benzyloxy)-2-oxoethyl)cyclopentylamino)-2-(biphenyl-4-ylmethyl)-4-oxobutanoate (93 mg); Retention time=1.85 minutes (condition B); MS (m+1)=590.3; 1H NMR (400 MHz, CDCl3, mixture of rotamers) δ ppm 1.61-1.72 (m, 6H) 1.96-2.06 (m, 2H) 2.17-2.46 (m, 2H) 2.81-3.00 (m, 4H) 3.22-3.29 (m, 1H) 5.02-5.12 (m, 4H) 5.62 (br s, 1H) 7.15-7.57 (m, 19H).

Aufarbeitung

  1. customthe reaction was quenched with H2O
  2. extractionThe product was extracted with EtOAc
  3. washthe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was purified by flash column chromatography on silica gel (eluent: heptane/EtOAc=100:0 to 0:100)

Quellen und Nachweise

ORD-Eintrag
ord-e094fd15efdf4a0b913cb90719f33af2
Quelldatensatz
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08877815B2

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