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RARECHEM AL BF 0026 synthesis

13synthesis methods
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Yield:20029-76-9 99%

Reaction Conditions:

Stage #1: asaronic acidwith sodium hydroxide in methanol; for 0.5 h;
Stage #2: methyl iodide in methanol at 50; for 5 h;

Steps:

1 Example:

(1) 2,4,5-trimethoxybenzoic acid (106 g, 0.5 mol),Sodium hydroxide (40 g, 1 mol) was added to 1500 mL of methanol.Stir for half an hour,62.3 mL of methyl iodide (1 mol) was slowly added dropwise at room temperature.After the addition is completed,The system was heated to 50 ° C and reacted for 5 hours, and the reaction was completed.The system was cooled to room temperature, concentrated under reduced pressure, and then added with water (2000 mL).Extraction with ethyl acetate (1500 mL x 3). Combine the organic phase,The organic phase is washed with water (2000 mL × 3), dried over anhydrous sodium sulfate, filtered,Concentration under reduced pressure gave Intermediate 2, yield: 99%.

References:

CN109608412,2019,A Location in patent:Paragraph 0026-0027