تفاعل #417225

معادلة التفاعل

Chloropropyltrimethoxysilane

1,1,1-trichloroethane

1-(2-aminoethyl)- piperazine

→

1-[2-[3-(trimethoxysilyl)- propyl]aminoethyl]piperazine

المردود 93.7%

ظروف التفاعل

المعالجة

1. 1
   أخرىA one-liter, four-necked flask was equipped with a thermometer
2. 2
   درجة الحرارةcooled to room temperature
3. 3
   ترشيحThe reaction mixture was rapidly filtered
4. 4
   أخرىto collect the 1-(2-aminoethyl)piperazine hydrochloride salt which
5. 5
   أخرىhad formed
6. 6
   workup.DISTILLATIONThe filtrate was distilled

الإجراء التجريبي

A one-liter, four-necked flask was equipped with a thermometer, a condensor, an inlet tube for nitrogen gas and an outlet tube for vent gases. Chloropropyltrimethoxysilane (198.72 g) was introduced into the flask, together with 50 g of anhydrrous 1,1,1-trichloroethane and 86.14 g of 1-(2-aminoethyl)- piperazine. The mixture was heated to 80° C. with continuous agitation for four hours and then cooled to room temperature. The reaction mixture was rapidly filtered to collect the 1-(2-aminoethyl)piperazine hydrochloride salt which had formed. The filtrate was distilled to yield 182 g of 1-[2-[3-(trimethoxysilyl)- propyl]aminoethyl]piperazine, bp 120°-143° C. at 10 mm Hg (69 kPa) as a pale yellow oil. The yield corresponded to 64% of theoretical. This material was used as an accelerator and adhesion promoter in the sealant compositions of this invention as detailed below in Example 5.

المصدر