反応 #4688

反応方程式

1-naphthol

sodium hydride

bromomalonic acid diethyl ester

→

α-naphthoxymalonic acid diethyl ester

溶媒

DMF

DMF

DMF

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture is further stirred for 16 hours at room temperature
2. 2
   濃縮concentrated by evaporation in a high vacuum
3. 3
   workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
4. 4
   洗浄washed with 2N sodium hydroxide solution, water and brine
5. 5
   乾燥dried over sodium sulphate
6. 6
   濃縮concentrated by evaporation
7. 7
   workup.DISTILLATIONThe residue is distilled at 145°-170°/2.6 Pa

実験手順

A solution of 25 g of 1-naphthol in 50 ml of DMF is slowly added dropwise to a solution of 7.6 g of sodium hydride dispersion in 300 ml of DMF. The suspension is stirred for 30 minutes and subsequently 41.5 g of bromomalonic acid diethyl ester in 50 ml of DMF are added dropwise. The reaction mixture is further stirred for 16 hours at room temperature and then concentrated by evaporation in a high vacuum. The residue is dissolved in ethyl acetate and washed with 2N sodium hydroxide solution, water and brine, dried over sodium sulphate and concentrated by evaporation. The residue is distilled at 145°-170°/2.6 Pa and yields α-naphthoxymalonic acid diethyl ester in the form of an orange-coloured oil.

出典