Iodine → Bis(thiobenzoyl) Disulfide

HRID 1636033

Reaktionsgleichung

Reaktionsgleichung von HRID 1636033
II.[Na+].[C:4]([S-:12])(=[S:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>C(OCC)C>[C:4]([S:12][S:12][C:4](=[S:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)(=[S:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Komponenten

4

Edukt 2

HCID 807IodineHCID 11030352Sodium dithiobenzoate

Produkt 1

HCID 10902862Bis(thiobenzoyl) DisulfideAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

An aqueous solution of iodine (1.0 N, 100 mL) was added dropwise to a stirred aqueous solution of dithiobenzoic acid sodium salt (0.1 mol in 100 mL of water) at room temperature over 15 minutes. Diethyl ether (100 mL) was added, the organic layer separated and washed twice with water, dried (Na2SO4), filtered and concentrated in vacuo. Di(thiobenzoyl)disulfide (7.5 g, 50%) was obtained after recrystallization from hot ethanol, m.p. 89-91° C. [lit(Houben, Chem, Ber., 39, 3219-3233, (1906). m.p. 92.5° C.]. 1H-nmr (CDCl3) δ (ppm) 7.44 (m, 4H, meta-ArH); 7.62 (m, 2H, para-ArH) and 8.11 (m, 4H, ortho-ArH).

Aufarbeitung

  1. customthe organic layer separated
  2. washwashed twice with water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-0b904497e7494475b98f17c298a9f463
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06512081B1

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