Methane → HCID 18916577, Verbindung

HRID 1290654Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1290654
[CH3:1][N:2]1[CH:10]2[CH:6]([CH2:7][C:8]([P:15]([OH:18])(=[O:17])[OH:16])([P:11]([OH:14])(=[O:13])[OH:12])[CH2:9]2)[CH2:5][CH2:4][CH2:3]1.[C:19]([S:22][CH2:23][CH2:24][Br:25])(=[O:21])[CH3:20].C>O.CS(C)=O>[Br-:25].[P:11]([C:8]1([P:15]([OH:16])([OH:18])=[O:17])[CH2:9][CH:10]2[CH:6]([CH2:5][CH2:4][CH2:3][N+:2]2([CH2:24][CH2:23][S:22][C:19](=[O:21])[CH3:20])[CH3:1])[CH2:7]1)([OH:12])([OH:14])=[O:13]

Komponenten

6

Edukt 3

HCID 297MethaneHCID 5230361-[(2-Bromoethyl)sulfanyl]ethan-1-oneHCID 14518763HCID 14518763, Verbindung

Produkt 1

HCID 18916577HCID 18916577, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Octahydro-1-methyl-1-pyrindine-6,6-diphosphonic acid (0.12 mmol) is dissolved in a mixture of water (25 ml) and DMSO (5 ml). To this is added 2-acetylthioethyl bromide (0.60 mmol) and the reaction mixture is heated at 60° for 24 hours. The reaction mixture is cooled, treated with charcoal, filtered and concentrated under reduced pressure. The crude residue is triturated with diethylether and the product can be obtained by recrystallizing the solid residue in water and isopropanol.

Aufarbeitung

  1. temperaturethe reaction mixture is heated at 60° for 24 hours
  2. temperatureThe reaction mixture is cooled
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude residue is triturated with diethylether
  6. customthe product can be obtained
  7. customby recrystallizing the solid residue in water

Quellen und Nachweise

ORD-Eintrag
ord-f301d39577144ce3ae58d6ad92ae7d2d
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05753634

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