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36097-42-4

AC-P-AMINO-PHE-OME synthesis

6synthesis methods
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Yield:36097-42-4 75.2%

Reaction Conditions:

with iron(0);ammonia hydrochloride;glacial acetic acid in ethanol;lithium hydroxide monohydrate at 90; for 3 h;

Steps:

1.4 (4) Preparation of (S)-methyl 2-acetamido-3-(4-aminophenyl) propionate (ie, a compound A5)

Reduced iron powder (11.1g, 0.199mol), ammonium chloride (0.68g, 0.013mol),Ethanol (56mL), water (14mL) and glacial acetic acid (3.4mL) were sequentially added to a 250mL three-necked flask equipped with a drying tube device, heated to 90°C for reflux reaction, mechanically stirred for 1.5h, (S)-Methyl 2-acetamido-3-(4-nitrophenyl) propionate (5.1 g, 0.019 mol) was added to continue the reaction for 3 h, suction filtered while hot, the filtrate was concentrated under reduced pressure, and dichloromethane ( 150mL), extract, add water (50mL×2) to wash, dry the organic phase over anhydrous magnesium sulfate for 4h; filter, and concentrate the filtrate under reduced pressure,3.4 g of yellow-white solid were obtained, yield: 75.2%.

References:

CN113845485,2021,A Location in patent:Paragraph 0048; 0059-0061

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