Hydrochloric Acid → H-Nva-Met-NH2.HCl

HRID 851723Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 851723
[NH:1](C(OC(C)(C)C)=O)[C@H:2]([C:6]([NH:8][C@H:9]([C:14]([NH2:16])=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=[O:7])[CH2:3][CH2:4][CH3:5].[ClH:24]>C(OCC)(=O)C.CCOCC>[NH2:1][C@H:2]([C:6]([NH:8][C@H:9]([C:14]([NH2:16])=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=[O:7])[CH2:3][CH2:4][CH3:5].[ClH:24]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 57006973BOC-Nva-Met-NH2

Produkt 1

HCID 88736758H-Nva-Met-NH2.HClAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

4.5 g (13 mmoles) of BOC-Nva-Met-NH2 are suspended in 20 ml of ethyl acetate, and 20 ml of a 6 n hydrochloric acid solution in ethyl acetate are added to the suspension. After one hour of standing the reaction mixture is diluted with ether, the separated precipitate is filtered off, and dried in vacuo over anhydrous sodium hydroxide. The resulting 4 g of crude product are recrystallized from a mixture of methanol and ether. 3.28 g (89%) of H-Nva-Met-NH2.HCl are obtained; m.p.: 198°-200° C., Rf5 =0.40, [α]D25 =+10.2° (c=1%, in methanol).

Aufarbeitung

  1. filtrationthe separated precipitate is filtered off
  2. dry with materialdried in vacuo over anhydrous sodium hydroxide
  3. customThe resulting 4 g of crude product are recrystallized from a mixture of methanol and ether

Quellen und Nachweise

ORD-Eintrag
ord-76928549785c412ea2c9bc34b93953ca
Quelldatensatz
uspto-grants-1983_05
Patentnummer
US04386073

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