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Dicyclohexylcarbodiimide → boc-D-Trp (+/-) trans-2,5-dicarbethoxypyrrolidine

HRID 1077672
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1077672
C1(N=C=NC2CCCCC2)CCCCC1.[C:16]([C@H:21]1[CH2:25][CH2:24][C@H:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[NH:22]1)([O:18][CH2:19][CH3:20])=[O:17].[C:31]([NH:38][C@@H:39]([C:50]([OH:52])=[O:51])[CH2:40][C:41]1[C:49]2[C:44](=[CH:45][CH:46]=[CH:47][CH:48]=2)[NH:43][CH:42]=1)([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32].O.ON1C2C=CC=CC=2N=N1>CN(C)C=O.C(OCC)(=O)C.C(Cl)(Cl)Cl.CO>[CH3:37][C:34]([O:33][C:31]([NH:38][C@@H:39]([C:50]([OH:52])=[O:51])[CH2:40][C:41]1[C:49]2[C:44](=[CH:45][CH:46]=[CH:47][CH:48]=2)[NH:43][CH:42]=1)=[O:32])([CH3:35])[CH3:36].[C:16]([C@H:21]1[CH2:25][CH2:24][C@H:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[NH:22]1)([O:18][CH2:19][CH3:20])=[O:17]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 10868Dicyclohexylcarbodiimide2×HCID 111050N-((tert-Butoxy)carbonyl)-D-tryptophanHCID 27960291-Hydroxybenzotriazole hydrateHCID 109109122,5-Diethyl (2R,5R)-pyrrolidine-2,5-dicarboxylate

Produkt 1

HCID 131719485boc-D-Trp (+/-) trans-2,5-dicarbethoxypyrrolidineAusbeute 115 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 21584188Chloroform methanolLösungsmittel

Versuchsvorschrift

3.9 g (19 mmol) of 1,3-dicyclohexylcarbodiimide (DCC) was added at 0° C. to a solution containing 1.63 g (7.58 mmol) of (±)-trans -2,5dicarbethoxypyrrolidine (1), 2.54 g (11 mmol) of Boc-D-tryptophan, 2.56 g (19 mmol) of 1-hydroxy benzotriazole hydrate, 3.3 ml (19 mmol) of diisopropyloethylamine in 25 ml of dry dimethylformamide (DMF). The resulting clear colorless solution was stirred under an argon atmosphere at room temperature for a period of 18 hr which resulted in the formation of a white precipitate. TLC analysis of the mixture (97:3 CHCl3 /MeOH) indicated that there was some remaining pyrrolidine diester. Therefore, an 2.0 g of DCC was added and the solution was stirred for an additional 5 hr at room temperature. Ethyl acetate (80 ml) was added to the reaction mixture and the solution was washed with water (3×25 ml) and brine solution (1×25 ml), and dried over MgSO4. Solvents were removed in vacuo and to produce 4.53 g of a thick yellow oil. Chromatography of the crude product on silica gel using the eluent showed that the product was a diastereomeric mixture (Rf=0.29 and 0.25) of the coupled products in an approximate ratio of 1.5:1. Total yield for both of the fractions containing the tryptophan pyrrolidine diester was 1.69 g (44.6%). The diastereomer possessing the higher Rf (0.29) was separated and analyzed yielding the following 1H NMR (CDCl3, 360 MHz) spectroscopic data:

Aufarbeitung

  1. customresulted in the formation of a white precipitate
  2. stirringthe solution was stirred for an additional 5 hr at room temperature
  3. washthe solution was washed with water (3×25 ml) and brine solution (1×25 ml)
  4. dry with materialdried over MgSO4
  5. customSolvents were removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-05ec79f2025d4555bb2d9b3d629e60d3
Quelldatensatz
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05543521

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