反応 #164104

反応方程式

ether

ethyl-4-oxocyclohexane carboxylate

ethylene glycol

→

raw product

収率 74.0%

1,4-dioxaspiro[4,5]decane-8-carboxylic acid ethyl ester

収率 74.0%

溶媒

toluol

反応条件

後処理

1. 1
   洗浄washed with water and 5% sodium hydrogencarbonate solution (150 mL each)
2. 2
   乾燥The organic phase was dried with sodium sulphate
3. 3
   濃縮concentrated to low volume in a vacuum

実験手順

A solution of ethyl-4-oxocyclohexane carboxylate (28.9 g, 169 mmol), ethylene glycol (36.7 g, 33.0 mL, 592 mmol) and p-toluol sulphonic acid (380 mg, 2.0 mmol) in toluol (90 mL) was stirred overnight at room temperature. The reaction solution was poured into ether (150 mL) and washed with water and 5% sodium hydrogencarbonate solution (150 mL each). The organic phase was dried with sodium sulphate and concentrated to low volume in a vacuum. Since the raw product (26.8 g) was obtained in pure form, it could be directly converted further.

出典