Water → 2-Thioxo-[1,3]dithiole-4-carboxylic acid methyl ester

HRID 1682092Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1682092
[S:1]1[C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4](C(OC)=O)[S:3][C:2]1=[S:14].O.[Br-].[Li+].O>CN(C)P(=O)(N(C)C)N(C)C>[S:3]1[CH:4]=[C:5]([C:6]([O:8][CH3:9])=[O:7])[S:1][C:2]1=[S:14]

Komponenten

5

Edukt 3

HCID 962WaterHCID 547914Dimethyl 2-thioxo-1,3-dithiole-4,5-dicarboxylateHCID 23702478Lithium bromide hydrate

Produkt 1

HCID 108671782-Thioxo-[1,3]dithiole-4-carboxylic acid methyl esterAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 12679HexamethylphosphoramideLösungsmittel

Versuchsvorschrift

30 Grams (0.12 mol) of dimethyl 1,3-dithiol-2-thion-4,5-dicarboxylate synthesized according to the method of G. C. Papavassiliou, et al [Synthetic Metals, Vol. 27 (1988) B-373-B378] was dissolved in 30 ml of hexamethylphosphorictriamide (HMPA), and 12.6 g (0.12 mol) of lithium bromide monohydrate was added. The resultant mixture was heated at 60° C. for 1 hour, the reaction mixture was allowed to cool to room temperature, 200 ml of water was added, and a yellow solid formed was separated by filtering and washed with water. The solid obtained was dried and recrystallized from carbon tetrachloride to give 16.2 g of yellow acicular crystals of methyl 1,3-dithiol-2-thione-4-carboxylate (yield 70%).

Aufarbeitung

  1. customa yellow solid formed
  2. customwas separated
  3. filtrationby filtering
  4. washwashed with water
  5. customThe solid obtained
  6. customwas dried
  7. customrecrystallized from carbon tetrachloride

Quellen und Nachweise

ORD-Eintrag
ord-f386a8c6f8bd459a858c1a15a2649769
Quelldatensatz
uspto-grants-1992_12
Patentnummer
US05175280

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