反応 #985268

ord-7bcb54a47354404383ce3f94e81486d4

反応方程式

[Na+].[OH-]
NaOH
CC1(C)OCC(CO)O1
1.2-isopropylidene-rac-glycerol
C=CCOCC1CO1
allyl glycidyl ether
CC(C)=C(O)C(O)CO
isopropylidene-rac-glycerol

溶媒

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGthe reaction mixture stirred for another 2 hours at 80° C

実験手順

A catalytic quantity of NaOH (MW 40.00; 0.6 mol-24 g) is added to 1.2-isopropylidene-rac-glycerol (MW 132.16; 16 mol-2115 g), which is rendered a solution by stirring and heating to 80° C. At 80° C., allyl glycidyl ether (MW 114.14; 6 mol-685 g) is added dropwise over a period of 2 hours, and the reaction mixture stirred for another 2 hours at 80° C. By this point in time the epoxide (Rf in ether=0.8) has reacted completely to form the G3 constituent (Rf in ether=0.6) The excess isopropylidene-rac-glycerol has an Rf of 0.65 in ether and is removed from the reaction mixture at 75° C./10 mbar. The residue has 1 l diisopropyl ether added to it and is extracted twice with 1 l NaCl (1% solution in H2O) in each case. The organic phase is rotated in an evaporator and distilled (Kpi10-1 mbar 125° C.).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07351428B2uspto-grants-2008_04