Methanol → Dicyclohexyl disulfide

HRID 255988

Reaktionsgleichung

Reaktionsgleichung von HRID 255988
CO.[OH-].[Na+].[CH:5]1([SH:11])[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.O=O>[Co].C([O-])(=O)C.[Co+2].C([O-])(=O)C.O>[CH:5]1([S:11][S:11][CH:5]2[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]2)[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1

Komponenten

8

Edukt 4

HCID 887MethanolHCID 977OxygenHCID 14798Sodium HydroxideHCID 15290Cyclohexanethiol

Produkt 1

HCID 17356Dicyclohexyl disulfideAusbeute 83,8 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6277Cobalt diacetateKatalysatorHCID 104730CobaltKatalysator2×HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
131 fahrenheit

Versuchsvorschrift

This example is an inventive run illustrating the use of another soluble cobalt-containing catalyst system. The run also suggests that because of the enhanced catalyst activity of the cobalt-containing catalyst system, the reaction can be operated with less alcohol present. Into a 300 milliliter stainless steel reactor equipped as described in Example I was charged 12 grams of methyl alcohol, 2 grams of sodium hydroxide, 0.1 gram of cobalt acetate and 86 grams (0.74) moles of cyclohexyl mercaptan. The reactor was pressured to 240 psig with nitrogen, heated to 55° C. (131° F.) and then pressured to 300 psig with oxygen. The reaction was complete in 3 hours. The effluent was water washed and the oil layer dried on a Rotovap at 90°-100° C./20-40 Torr. (mm) to give a 100 percent selectivity and 83.8 percent yield of dicyclohexyl disulfide.

Aufarbeitung

  1. additioncontaining catalyst system
  2. additioncontaining catalyst system
  3. customthe reaction
  4. customInto a 300 milliliter stainless steel reactor equipped
  5. washwashed
  6. customthe oil layer dried on a Rotovap at 90°-100° C./20-40 Torr

Quellen und Nachweise

ORD-Eintrag
ord-3595b63384464fec8d4f90434d849f5e
Quelldatensatz
uspto-grants-1987_10
Patentnummer
US04700004

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