Carbon Disulfide → Antimony N-(2-octyl)-N-ethyldithiocarbamate

HRID 1288403

Reaktionsgleichung

Reaktionsgleichung von HRID 1288403
[CH3:1][CH:2]([NH:9][CH2:10][CH3:11])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].O=[Sb:13]O[Sb]=O.CCCCCC.[C:23](=[S:25])=[S:24]>O>[CH3:1][CH:2]([N:9]([CH2:10][CH3:11])[C:23](=[S:24])[S-:25])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[Sb+3:13].[CH3:1][CH:2]([N:9]([CH2:10][CH3:11])[C:23](=[S:24])[S-:25])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH3:1][CH:2]([N:9]([CH2:10][CH3:11])[C:23](=[S:24])[S-:25])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

Komponenten

6

Edukt 4

HCID 6348Carbon DisulfideHCID 8058HexaneHCID 27652Oxo(oxostibanyloxy)stibaneHCID 5250531-Heptanamine, 1-methyl, N-ethyl

Produkt 1

HCID 21501793Antimony N-(2-octyl)-N-ethyldithiocarbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
68 °C

Versuchsvorschrift

In a 3-liter, three-neck, round-bottom flask equipped with a stirrer, thermometer, dropping funnel and condenser was placed 157 g. (grams) (1.0 mole) of N-(2-octyl)-N-ethylamine, 49 g. (0.168 mole) of antimony trioxide and 1000 ml. (milliliters) of hexane. The stirred mixture was heated to reflux (68°C.) and 80 g. (1.05 moles) of carbon disulfide was added over a period of 1 hour. The mixture was stirred at reflux for an additional 3 hours, and then the water generated during the reaction was azeotroped off (9 ml.). The mixture was filtered hot in order to remove any unreacted antimony oxide. The hexane solution was cooled to room temperature and the hexane was then removed at reduced pressure. A viscous oil was isolated having an Index of refraction ND22 =1.627.

Aufarbeitung

  1. customIn a 3-liter, three-neck, round-bottom flask equipped with a stirrer
  2. temperatureThe stirred mixture was heated
  3. temperatureat reflux for an additional 3 hours
  4. customwas azeotroped off (9 ml.)
  5. filtrationThe mixture was filtered hot in order
  6. customto remove any unreacted antimony oxide
  7. temperatureThe hexane solution was cooled to room temperature
  8. customthe hexane was then removed at reduced pressure
  9. customA viscous oil was isolated

Quellen und Nachweise

ORD-Eintrag
ord-ee4a5f3811d6448da4ab0885712207dd
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03988249

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