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1 5-DIACETYLINDOLINE 97 synthesis

2synthesis methods
-

Yield:16078-35-6 88%

Reaction Conditions:

with Aluminum Chloride in dichloromethane; for 16 h;Inert atmosphere;Reflux;

Steps:

1 Synthesis of 1,5-Diacetylindoline (1B)

1A (6.60 g, 40.94 mmol) was dissolved in 25 mL of anhydrous dichloromethane, anhydrous aluminum chloride (16.38 g, 122.83 mmol) was added at 0° C. under nitrogen atmosphere, and acetyl chloride (4.82 g, 61.41 mmol) was slowly added dropwise. ) in anhydrous dichloromethane (10 mL), removed the ice bath after half an hour, refluxed for 16 h, quenched with water (70 mL) under ice bath, extracted with dichloromethane (3×60 mL), combined the organic phases, saturated brine Washed, dried over anhydrous magnesium sulfate, filtered with suction, concentrated under reduced pressure, and separated and purified by column chromatography to obtain 7.32 g of a yellow solid with a yield of 88.0%

References:

CN114213310,2022,A Location in patent:Paragraph 0068-0069; 0072-0073