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Hydrochloric Acid → HCID 178512901, Verbindung

HRID 1414682
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1414682
[NH:1](C(OCC1C=CC=CC=1)=O)[C@H:2]([C:13]([N:15]1[CH2:56][CH2:55][CH2:54][C@H:16]1[C:17]([NH:19][C@H:20]([C:28]([NH:30][C@H:31]([C:39]([NH:41][C@H:42]([C:51]([NH2:53])=[O:52])[CH2:43][C:44]1[CH:49]=[CH:48][C:47]([OH:50])=[CH:46][CH:45]=1)=[O:40])[CH2:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=[O:29])[CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:18])=[O:14])[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[NH:12])[NH:8][N+]([O-])=O.Cl.N[C@H](C(O)=O)CCCNC(=N)N.N[C@H](C(O)=O)CC1C=CC(O)=CC=1.N[C@H](C(O)=O)CC1C=CC=CC=1>[Pd].O.C(O)(=O)C>[NH2:1][C@H:2]([C:13]([N:15]1[CH2:56][CH2:55][CH2:54][C@H:16]1[C:17]([NH:19][C@H:20]([C:28]([NH:30][C@H:31]([C:39]([NH:41][C@H:42]([C:51]([NH2:53])=[O:52])[CH2:43][C:44]1[CH:49]=[CH:48][C:47]([OH:50])=[CH:46][CH:45]=1)=[O:40])[CH2:32][C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1)=[O:29])[CH2:21][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)=[O:18])=[O:14])[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[NH:8])[NH2:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 313Hydrochloric AcidHCID 6057L-TyrosineHCID 6140L-PhenylalanineHCID 178418600HCID 178418600, VerbindungHCID 178512178HCID 178512178, Verbindung

Produkt 1

HCID 178512901HCID 178512901, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

In 30 ml. of acetic acid was dissolved 500 mg. of Z-Arg(NO2)-Pro-Phe-Phe-Tyr-NH2, and catalytic reduction was carried out with Pd-black as a catalyst for 20 hours. The catalyst was filtered off and the filtrate was concentrated to dryness under reduced pressure. The residue was dissolved in 50 ml. of water and, after the small amounts of insolubles were filtered off, the filtrate was lyophilized. The product was dissolved in 5 ml. of water and the solution was applied on a column (1.8 × 9 cm) of carboxymethyl-sephadex. Gradient elution was carried out with 0.1M aqueous ammonium acetate (400 ml.) and 1M aqueous ammonium acetate (400 ml.). The fractions from 250 ml. to 370 ml. were pooled and lyophilized to yield 250 mg. (52.3 %) of a white fluffy product. [α]D24 -41.9° (c=0.47 %, water). Amino acid analysis (hydrolysis with HCl): Arg, 1.00;Pro, 1.05; Tyr, 0.91; Phe, 1.96;(peptide content 86.5 %).

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated to dryness under reduced pressure
  3. dissolutionThe residue was dissolved in 50 ml
  4. filtrationof water and, after the small amounts of insolubles were filtered off
  5. dissolutionThe product was dissolved in 5 ml
  6. washGradient elution
  7. customto yield 250 mg

Quellen und Nachweise

ORD-Eintrag
ord-68c06e1ab20c47c3aea036b125c822ac
Quelldatensatz
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04001199

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