Methanol → Dicyclohexyl disulfide

HRID 255988

反応式

HRID 255988 の反応式
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

参加物

8

反応物 4

HCID 887MethanolHCID 977OxygenHCID 14798Sodium HydroxideHCID 15290Cyclohexanethiol

生成物 1

HCID 17356Dicyclohexyl disulfide収率 83.8%

試薬・触媒・溶媒 3

HCID 6277Cobalt diacetate触媒HCID 104730Cobalt触媒2 回HCID 962Water溶媒

反応条件

温度
131 fahrenheit

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3595b63384464fec8d4f90434d849f5e
出典データセット
uspto-grants-1987_10
特許番号
US04700004

関連ノート

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