反応 #335286

反応方程式

sulfuric acid

acrylic acid

sodium hydroxide

n-octylmercaptan

→

3-octylthiopropionic acid

収率 98.6%

溶媒

water

water

isopropyl alcohol

反応条件

後処理

1. 1
   workup.ADDITIONwas added to a vessel
2. 2
   その他proceeded at 50° to 60° C
3. 3
   温度to reflux for 2 hours
4. 4
   温度After cooling to 55° C.
5. 5
   workup.ADDITIONby pouring into a separatory device
6. 6
   洗浄the organic layer was washed with an equal volume of water containing 2% sodium sulfate
7. 7
   その他at 60° C.

実験手順

A charge of 1.00 mole of n-octylmercaptan in an isopropyl alcohol and water 1:1 blend was added to a vessel. At room temperature, 1.16 mole of sodium hydroxide in an equal volume of water was added to the vessel, and an exotherm proceeded at 50° to 60° C. Over a 30-minute period, 1.05 mole of acrylic acid was added dropwise, the temperature was then raised to 85° C., and the mixture was allowed to reflux for 2 hours. After cooling to 55° C., 70% aqueous sulfuric acid (0.59 mole) was added, with stirring for 30 minutes, followed by pouring into a separatory device. The aqueous layer was drained off, and the organic layer was washed with an equal volume of water containing 2% sodium sulfate. After vacuum stripping at 60° C., the reaction product was analyzed to contain 0.04% octylmercaptan and a yield of 98.6% of 3-octylthiopropionic acid product.

出典