Hydrogen Sulfide → HCID 178523350, Verbindung

HRID 462395

Reaktionsgleichung

Reaktionsgleichung von HRID 462395
C(N(CC)CC)C.ClC(OCC(C)C)=O.[N+:16]([C:19]1[CH:35]=[CH:34][C:22]([CH2:23][O:24][C:25]([NH:27][CH2:28][CH2:29][CH2:30][C:31](O)=[O:32])=[O:26])=[CH:21][CH:20]=1)([O-:18])=[O:17].S.[S:37](=O)(=O)(O)O>C(Cl)Cl>[N+:16]([C:19]1[CH:35]=[CH:34][C:22]([CH2:23][O:24][C:25]([NH:27][CH2:28][CH2:29][CH2:30][C:31]([OH:32])=[S:37])=[O:26])=[CH:21][CH:20]=1)([O-:18])=[O:17]

Komponenten

7

Edukt 5

HCID 402Hydrogen SulfideHCID 1118Sulfuric AcidHCID 8471TriethylamineHCID 62365Isobutyl chloroformateHCID 31025414-(p-Nitrobenzyloxycarbonyl)aminobutyric acid

Produkt 1

HCID 178523350HCID 178523350, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

2.2 g (20 mmol) of triethylamine and a solution of 1.4 ml (10 mmol) of isobutyl chloroformate in 20 ml of dry methylene chloride are added dropwise in succession to a solution, cooled to -10°, of 2.82 g (10 mmol) of 4-p-nitrobenzyloxycarbonylaminobutyric acid in 50 ml of dry methylene chloride. The reaction mixture is stirred for one hour and subsequently a strong current of hydrogen sulphide is passed through for a period of 2 hours. After acidifying with 2N sulphuric acid, the organic phase is separated, dried and concentrated in vacuo. The 4-p-nitrobenzyloxycarbonylaminothiobutyric acid obtained can be used without further purification.

Aufarbeitung

  1. customis passed through for a period of 2 hours
  2. customthe organic phase is separated
  3. customdried
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-61ae72628f5d41f9854cd91a591bf4bb
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04515717

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