反応 #89598

反応方程式

Diethyl phosphite

product

2-(1,3-oxazolidin-3-yl)ethanol

→

diethyl [bis(2-hydroxyethyl)amino]methylphosphonate

反応条件

後処理

1. 1
   その他to form a reaction mixture
2. 2
   workup.ADDITIONOn completion of the addition
3. 3
   温度to cool to a temperature of 25° C
4. 4
   抽出The product was extracted with a 2:1 mixture of diethyl ether and ethyl acetate (5×300 ml)
5. 5
   乾燥the combined extracts were dried over magnesium sulphate
6. 6
   その他evaporated

実験手順

Diethyl phosphite (2.5 mol, 352/3 g) was added slowly to a mixture of the product from stage (1.1) and Amberlight™ IR120 resin—acid form (available from Aldrich, 100 g) to form a reaction mixture. On completion of the addition, the reaction mixture was stirred at 60° C. for 2 hours and then allowed to cool to a temperature of 25° C. The product was extracted with a 2:1 mixture of diethyl ether and ethyl acetate (5×300 ml), the combined extracts were dried over magnesium sulphate and evaporated to give 354 g of diethyl [bis(2-hydroxyethyl)amino]methylphosphonate in the form of a pale yellow liquid. The product was stored over 4A molecular sieves. This was designated Monomer (1).

出典