1H-Isoindole-1,3(2H)-dione, 2-[4-[(6-methoxy-8-quinolinyl)amino]pentyl]- synthesis
- Product Name:1H-Isoindole-1,3(2H)-dione, 2-[4-[(6-methoxy-8-quinolinyl)amino]pentyl]-
- CAS Number:83532-78-9
- Molecular formula:C23H23N3O3
- Molecular Weight:389.45
Yield:83532-78-9 90.4%
Reaction Conditions:
with sodium carbonate in toluene at 140 - 150; for 0.333333 h;
Steps:
4-6 Synthesis of dicondensate (BAK-Z2)
Add 296.2g of monocondensate, 418g of 6-methoxy-8-aminoquinoline and 106g of sodium carbonate into the reaction vessel. The molar ratio of monocondensate to 6-methoxy-8-aminoquinoline and sodium carbonate is 1:2.4:1. Stir, heat up to 140-150°C and keep the reaction warm. After the reaction, add 2500ml of toluene while it is hot, stir for 20min, and filter to obtain the dicondensate toluene solution. Add 15 g of activated carbon to the filtrate, stir to decolorize, filter, and wash with toluene.Add the 1% sulfuric acid solution prepared in advance to the above toluene solution in portions for pickling. For the first pickling, add 145g of 1% sulfuric acid solution, and then 80g each time, stirring and pickling at 65-70. Thermal stratification, the water layer is used to recover 6-methoxy-8-aminoquinoline, the upper organic layer is repeatedly washed with sulfuric acid aqueous solution to reach the end point (end point judgment method: take 5mL acid aqueous solution, add 1.5% sulfuric acid aqueous solution 3mL, Then add 1 drop of 0.1N sodium nitrite solution, apply potassium iodide starch reagent on the white magnetic plate, and reach the end point if it turns blue), collect the water layer for recovery of unreacted aminoquinoline. The organic layer was washed twice with water, dried with 50 g of anhydrous sodium sulfate, filtered, and the filtrate was distilled to recover toluene to obtain 352 g of dicondensate, with a yield of 90.4% and a theoretical amount of 389.46 g.
References:
CN113248431,2021,A Location in patent:Paragraph 0039-0052
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