反応 #217450

反応方程式

triethanolamine

isatoic anhydride

1,4-diazabicyclo(2.2.2)octane

dimethylformamide

→

beige solid

収率 90.3%

Triethanolamine Trianthranilate

収率 90.3%

溶媒

methanol

water

反応条件

後処理

1. 1
   その他Into a 1 liter round bottom flask-equipped with mechanical stirrer
2. 2
   温度The mixture was then cooled to room temperature
3. 3
   workup.STIRRINGThis solution was stirred for 2 hours
4. 4
   ろ過filtered
5. 5
   洗浄washed with 5×250 milliliters of methanol, and oven
6. 6
   その他dried at 60° C.

実験手順

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.

出典