Ethylenediamine → (Trimethoxysilylpropyl)ethylenediamine

Participants

Reaction Steps

A 300-ml, four necked glass flask equipped with a stirrer, reflux condenser, and thermometer was charged with 180.0 g (3.0 mol) of ethylene diamine and heated at 80° to 90° C. From a dropping funnel, 74.4 g (0.37 mol) of 3-chloropropyltrimethoxysilane was added dropwise to the flask over 1.25 hours (the molar ratio of ethylene diamine/3-chloropropyltrimethoxysilane=8.11). After one hour ripening, thereaction solution was heated until boiling whereupon 82.3 g (1.37 mol) of ethylene diamine was distilled out of the system through a reflux outlet port. The concentrated reaction solution was transferred to a separatory funnel and cooled for allowing the solution to separate into two layers. The lower layer of ethylene diamine hydrochloride was separated off. The upper layer containing 3-[N-(2-aminoethyl)]aminopropyltrimethoxysilane wastaken out and purified by simple distillation, obtaining 67.2 g of 3-[N-(2-aminoethyl)]aminopropyltrimethoxysilane. The yield was 81.7%.

Provenance & Evidence