反応 #1241931

反応方程式

potassium octane-1-thiolate

n-oct-1-yl mercaptan

potassium methylate

methanol

→

n-octyl methyl sulfide

収率 92.0%

溶媒

反応条件

後処理

1. 1
   その他The carbon monoxide consumed during the reaction
2. 2
   workup.DISTILLATIONwas distilled under atmospheric pressure
3. 3
   その他a methanol/methyl formate mixture was separated off

実験手順

In a 0.3 liter stainless steel stirred autoclave, 37.9 g (0.26 mole) of n-oct-1-yl mercaptan and 20.3 g (0.29 mole) of potassium methylate were dissolved in 120 ml (3.0 moles) of methanol at 20° C., the resulting potassium octane-1-thiolate solution was heated from 20° to 150° C. in the course of 20 minutes under a carbon monoxide pressure of 300 bar, and the mixture was then kept at this temperature for 15 hours. The carbon monoxide consumed during the reaction was replaced continuously, and the pressure was kept constant at 300 bar. The mixture which emerged from the reactor was distilled under atmospheric pressure, and a methanol/methyl formate mixture was separated off and 38.2 g (92% of theory) of n-octyl methyl sulfide was obtained at 110° C./34 mbar.

出典