反应 #576141

反应方程式

1-dodecylbenzene

diisopropylethylamine

hydrochloric acid

aluminum chloride

benzene-1,2,4,5-tetracarboxylic acid dianhydride

→

2,5-bis(4-dodecylbenzoyl)terephthalic acid

溶剂

1,2-dichloroethane

1,2-dichloroethane

water

ethyl acetate

tetrahydrofuran

反应条件

后处理

1. 1
   其他the temperature between 15° C. and 20° C.
2. 2
   workup.ADDITIONduring the addition
3. 3
   workup.STIRRINGThe mixture was stirred for one hour
4. 4
   workup.ADDITIONthe liquid was poured from the coagulate
5. 5
   workup.STIRRINGThe mixture was stirred
6. 6
   其他phase split
7. 7
   过滤The organic phase was filtered
8. 8
   浓缩the filtrate was concentrated in vacuo
9. 9
   workup.ADDITIONTo 127 grams of the combined residue was added 800 mL of ethyl acetate
10. 10
    workup.STIRRINGthe resulting mixture was stirred until a suspension of a fine solid
11. 11
    其他resulted
12. 12
    过滤The solid was collected by filtration
13. 13
    洗涤washed with 50 mL of ethyl acetate
14. 14
    其他The solid was dried

实验过程

To a mixture of 492 grams of aluminum chloride and 988 mL of 1,2-dichloroethane was added 192 grams of benzene-1,2,4,5-tetracarboxylic acid dianhydride (pyromellitic dianhydride). The resulting mixture was cooled to 16° C. and a solution of 434 grams of 1-dodecylbenzene, 123 grams of diisopropylethylamine and 480 mL of 1,2-dichloroethane was added over a period of 3.5 hours, keeping the temperature between 15° C. and 20° C. during the addition. The mixture was stirred overnight at room temperature and poured into a beaker of 1000 grams of ice and 1000 grams concentrated hydrochloric acid. The mixture was stirred for one hour and the liquid was poured from the coagulate. The mixture was divided into 800 mL portions and each portion was worked up as follows. To 800 mL of the mixture was added 800 mL of tetrahydrofuran, 800 mL of ethyl acetate and 800 mL of water. The mixture was stirred and phase split. The organic phase was filtered and the filtrate was concentrated in vacuo. The resulting residues were combined. To 127 grams of the combined residue was added 800 mL of ethyl acetate and the resulting mixture was stirred until a suspension of a fine solid resulted. The solid was collected by filtration and washed with 50 mL of ethyl acetate. The solid was dried to give 2,5-bis(4-dodecylbenzoyl)terephthalic acid.

来源