1,4-Dibromo-2,3-butanediol → HCID 86752373, Verbindung

HRID 1275415

Reaktionsgleichung

Reaktionsgleichung von HRID 1275415
Br[CH2:2][CH:3]([OH:8])[CH:4]([OH:7])[CH2:5]Br.[OH2:9].[OH2:10].O.O.O.O.O.O.O.O.O.O.[P:21]([O-:25])([O-:24])([O-:23])=[S:22].[Na+].[Na+].[Na+]>CN(C=O)C.O.[N+]([O-])([O-])=O.[Ag+]>[OH2:7].[OH2:23].[OH2:9].[OH2:7].[P:21](=[S:22])([OH:25])([OH:24])[OH:23].[P:21](=[S:22])([OH:25])([OH:24])[OH:23].[CH2:2]([OH:10])[C@H:3]([C@@H:4]([CH2:5][OH:9])[OH:7])[OH:8]

Komponenten

6

Edukt 2

HCID 985121,4-Dibromo-2,3-butanediolHCID 45052183Sodium phosphorothioate hydrate (3:1:12)

Produkt 1

HCID 86752373HCID 86752373, VerbindungAusbeute 285 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24470Silver NitrateKatalysatorHCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 1,4-dibromo-2,3-butanediol (1.0 g, 4.0 mmol) in 5 ml DMF is added to sodium thiophosphate dodecahydrate (3.8 gm, 10.1 mmol) in 20 ml H2O. The mixture is stirred overnight at room temperature. A 5% silver nitrate solution is added to precipitate excess sodium thiophosphate. The precipitate is filtered out and the filtrate dried under high vacuum. The solid residue is triturated with methanol and filtered to yield 1.8 g (3.8 mmol) of threitol bis-phosphorothioate tetrahydrate.

Aufarbeitung

  1. customto precipitate excess sodium thiophosphate
  2. filtrationThe precipitate is filtered out
  3. customthe filtrate dried under high vacuum
  4. customThe solid residue is triturated with methanol
  5. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-2d5564b47fef4cd8bd37db7b1ab47034
Quelldatensatz
uspto-grants-2000_12
Patentnummer
US06160153

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