반응 #217450

반응 방정식

triethanolamine

isatoic anhydride

1,4-diazabicyclo(2.2.2)octane

dimethylformamide

→

beige solid

수율 90.3%

Triethanolamine Trianthranilate

수율 90.3%

용매

methanol

water

반응 조건

후처리

1. 1
   기타Into a 1 liter round bottom flask-equipped with mechanical stirrer
2. 2
   온도The mixture was then cooled to room temperature
3. 3
   workup.STIRRINGThis solution was stirred for 2 hours
4. 4
   여과filtered
5. 5
   세척washed with 5×250 milliliters of methanol, and oven
6. 6
   기타dried at 60° C.

실험 절차

Into a 1 liter round bottom flask-equipped with mechanical stirrer, dropping funnel, and thermometer was charged triethanolamine (149.2 grams, 1.0 mol; obtained from Sigma-Aldrich), isatoic anhydride (520.0 grams, 3.5 mol), 1,4-diazabicyclo(2.2.2)octane (DABCO) (45.0 grams, 0.4 mol), and dimethylformamide (1,500 milliliters). The mixture was stirred and heated to 120° C. for a period of about 2 hours. The mixture was then cooled to room temperature, and methanol (2 liters) was added. Deionized water (1 liter) was added, causing the solution to turn cloudy. This solution was stirred for 2 hours, and then filtered, washed with 5×250 milliliters of methanol, and oven dried at 60° C. to yield 506 grams of a beige solid.

출처