反应详情

温度

120 °C

A one liter, four necked, round bottom flask, equipped with an overhead stirrer, sub-surface gas inlet tube, thermowell, Dean-Stark trap, and Friedrick's condenser, is charged with 313.4 grams (1.56 moles) of 2,4,6,8-tetramethyl-nonan-1-ol. The flask is purged with nitrogen and warmed to 120 degrees C. 3.7 grams (46 mmoles) of a 50 percent by weight solution of NaOH in water is added drop-wise over 1 minute. The mixture is stirred at 120 degrees C. for 1 hour and water is collected in the Dean-Stark trap. 250 grams of isatoic anhydride (1.53 moles) is added portion-wise, supra-surface, over a period of 50 minutes. The mixture is stirred at 145 degrees C. for 6 hours. 9 grams of Fax-5 filter aid is added to the flask and stirred. The mixture is filtered and cooled to yield 456 grams of the product, in the form of a brown liquid. The product has a TBN, by ASTM D2896, of 150.

1. customA one liter, four necked, round bottom flask, equipped with an overhead stirrer, sub-surface gas inlet tube
2. customThe flask is purged with nitrogen
3. addition3.7 grams (46 mmoles) of a 50 percent by weight solution of NaOH in water is added drop-wise over 1 minute
4. customwater is collected in the Dean-Stark trap
5. waitsupra-surface, over a period of 50 minutes
6. stirringThe mixture is stirred at 145 degrees C
7. waitfor 6 hours
8. addition9 grams of Fax-5 filter aid is added to the flask
9. stirringstirred
10. filtrationThe mixture is filtered
11. temperaturecooled