Water → L-methionyl-L-aspartyl-D-alanine amide hydrochloride

HRID 596804Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 596804
C(OC([NH:8][C@H:9]([C:14]([NH:16][C@H:17]([C:22]([NH:24][C@@H:25]([C:27]([NH2:29])=[O:28])[CH3:26])=[O:23])[CH2:18][C:19](=[O:21])[OH:20])=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=O)(C)(C)C.O.[ClH:31].O1CCOCC1>C(O)(=O)C>[ClH:31].[NH2:8][C@H:9]([C:14]([NH:16][C@H:17]([C:22]([NH:24][C@@H:25]([C:27]([NH2:29])=[O:28])[CH3:26])=[O:23])[CH2:18][C:19](=[O:20])[OH:21])=[O:15])[CH2:10][CH2:11][S:12][CH3:13]

Komponenten

5

Edukt 3

HCID 962WaterHCID 204431481,4-Dioxane hydrochlorideHCID 22796339N-t-butoxycarbonyl-L-methionyl-L-aspartyl-D-alanine amide

Produkt 1

HCID 22796354L-methionyl-L-aspartyl-D-alanine amide hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

12.54 Parts of N-t-butoxycarbonyl-L-methionyl-L-aspartyl-D-alanine amide is dissolved in 107 parts by volume glacial acetic acid and 51.66 parts by volume of a 5.6 M solution of HCl/dioxane. The resultant mixture is stirred for 20 minutes and then stripped under reduced pressure to afford a solid. The solid is triturated with ethyl ether, cooled, and the resultant product washed with cold ethyl ether and vacuum dried. This solid is purified by countercurrent distribution to afford L-methionyl-L-aspartyl-D-alanine amide hydrochloride hydrated with 2/3 mole of water per mole, and represented by the following formula.

Aufarbeitung

  1. customto afford a solid
  2. customThe solid is triturated with ethyl ether
  3. temperaturecooled
  4. washthe resultant product washed with cold ethyl ether and vacuum
  5. customdried
  6. customThis solid is purified by countercurrent distribution

Quellen und Nachweise

ORD-Eintrag
ord-c6ddfcbe70fe4dab9a37bb9b849a37d2
Quelldatensatz
uspto-grants-1977_03
Patentnummer
US04012367

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