Disalicylimide synthesis
- Product Name:Disalicylimide
- CAS Number:1972-71-0
- Molecular formula:C14H11NO4
- Molecular Weight:257.24
Yield: 90%
Reaction Conditions:
Stage #1:salicylic acid with thionyl chloride in N,N-dimethyl-formamide;toluene at 50; for 2 h;
Stage #2:salicylamide with 1,8-diazabicyclo[5.4.0]undec-7-ene in N,N-dimethyl-formamide;toluene;acetonitrile at 5; for 24 h;
Stage #3: with hydrogenchloride in water;N,N-dimethyl-formamide;toluene;acetonitrile at 20; for 2 h;
Steps:
m1
Salicylic acid (300 g) was suspended in 600 mL of toluene and after adding 258 g of thionyl chloride and 7 mL of DMF thereto, the mixture was stirred at 50°C for 2 hours (Solution A). To a solution obtained by adding and dissolving 900 mL of acetonitrile and 660 g of DBU (diazabicycloundecene (1,8-diazabicyclo[5.4.0]undec-7-ene)) in 299.0 g of salicylamide, Solution A prepared above was added dropwise under the condition of 5°C, and the mixture was stirred at room temperature for 24 hours. To the resulting reaction solution, 300 mL of 35% hydrochloric acid was added, and the mixture was stirred at room temperature for 2 hours. The obtained solid was filtered and washed with water to obtain 504 g of Synthetic Intermediate mA (yield: 90%).
References:
FUJIFILM Corporation EP2460799, 2012, A1 Location in patent:Page/Page column 40
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