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L-Pyroglutamic Acid → (S)-2-benzylcarbamoyl-5-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester

HRID 73499
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 73499
C1(N=C=NC2CCCCC2)CCCCC1.[NH:16]1[C:20](=[O:21])[CH2:19][CH2:18][C@H:17]1[C:22]([OH:24])=O.[CH2:25]([NH2:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.[C:33](OC([O-])=O)([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34].C(N(CC)CC)C>CN(C)C=O.CN(C)C1C=CN=CC=1>[C:36]([O:35][C:33]([N:16]1[C:20](=[O:21])[CH2:19][CH2:18][C@H:17]1[C:22](=[O:24])[NH:32][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:34])([CH3:39])([CH3:38])[CH3:37]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 7405L-Pyroglutamic AcidHCID 7504BenzylamineHCID 8471TriethylamineHCID 10868DicyclohexylcarbodiimideHCID 22064466Tert-butyldicarbonate

Produkt 1

HCID 71114834(S)-2-benzylcarbamoyl-5-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester
Ausbeute 17,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

N,N′-Dicyclohexyl carbodiimide (DCC; 8.2 g, 40 mmol) was added to a solution of pyroglutamic acid (5.16 g, 40 mmol) in dimethylformamide (DMF; 60 ml). The mixture was stirred at room temperature for 2 h and a precipitate formed. Benzylamine (4.8 ml, 44 mmol) was added and the mixture was stirred for 2 h. t-butyl dicarbonate (Boc2O; 9.6 g, 44 mmol), triethylamine (TEA; 6.3 ml, 44 mmol) and 4-dimethylaminopyridine (DMAP; 488 mg, 4 mmol) were added and the mixture was stirred at room temperature for 16 h. The DMF was removed under vacuum and the residue was taken up with water (20 ml) and extracted with dichloromethane (DCM; 3×20 ml). The organic layers were concentrated and the crude product was purified via silica gel chromatography to afford (S)-2-benzylcarbamoyl-5-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester (2.23 g, 7.0 mmol, 17.5%).

Aufarbeitung

  1. customa precipitate formed
  2. additionwere added
  3. stirringthe mixture was stirred at room temperature for 16 h
  4. customThe DMF was removed under vacuum
  5. extractionextracted with dichloromethane (DCM; 3×20 ml)
  6. concentrationThe organic layers were concentrated
  7. customthe crude product was purified via silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-c29b893a97a54d9590df659b272e770b
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08829191B2

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