反応 #94328

反応方程式

benzene

2,6,6-trimethylcyclohex-2-en-1,4-dione

propylene glycol

→

product

収率 80.0%

2,7,9,9-Tetramethyl-1,4-Dioxaspiro[4,5]Dec-6-En-8-One

収率 80.0%

溶媒

water

water

反応条件

後処理

1. 1
   その他To a 2-liter flask fitted with a reflux condenser
2. 2
   その他prepared by the method
3. 3
   その他is collected in the water separator
4. 4
   洗浄The product is washed with water to a pH of 6
5. 5
   workup.DISTILLATIONdistilled through a 9 inch Goodloe column

実験手順

To a 2-liter flask fitted with a reflux condenser, a water separator and a stirrer is charged 265 g of 2,6,6-trimethylcyclohex-2-en-1,4-dione (prepared by the method described in Helv. Chim. Acta, 39:2041 [1956]), 266 g of propylene glycol, 500 ml of benzene and 1 g of p-toluenesulfonic acid. The reactants are stirred and refluxed until no additional water is collected in the water separator. The product is washed with water to a pH of 6, and the solvent is stripped off. The residue is vacuum distilled through a 9 inch Goodloe column to yield 257 g of product, boiling point 92° C. at 1 mm Hg (80% yield).

出典