diethyl 2-(1-(4-acetaMidophenyl)-1-oxopropan-2-yl)Malonate synthesis
- Product Name:diethyl 2-(1-(4-acetaMidophenyl)-1-oxopropan-2-yl)Malonate
- CAS Number:81937-39-5
- Molecular formula:C18H23NO6
- Molecular Weight:349.38
![N-[4-(2-CHLOROPROPANOYL)PHENYL]ACETAMIDE](/StructureFile/ChemBookStructure8/GIF/CB6298528.gif)
81112-08-5
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81937-39-5
Example A29: Diethyl malonate (0.16 mol) was slowly added dropwise to a suspension of anhydrous dimethylformamide (90 mL) containing sodium hydride (7.631 g, 0.159 mol) under nitrogen protection. The reaction mixture was heated to 50 °C and maintained for 90 minutes. Subsequently, 1-(4-acetylaminophenyl)-2-chloro-1-propanone (37.462 g, 0.166 mol) was added to the reaction system and the temperature was raised to 80 °C to continue the reaction for 3 hours. Upon completion of the reaction, the mixture was cooled and poured into ice water (1 L), washed with saturated sodium chloride solution, followed by full extraction with ethyl acetate. The organic phases were combined, dried with anhydrous sodium sulfate, filtered and treated with activated carbon and finally concentrated under reduced pressure. The crude product was purified by silica gel column chromatography to give 45.0 g of a colorless oily product in 80% yield with an Rf value of 0.7 (El:EE).IR (KBr) showed absorption peaks at 1747, 1732, 1676 cm^-1 (CO). Mass spectrometry analysis showed a molecular ion peak M+ of 349.
![N-[4-(2-bromopropanoyl)phenyl]acetamide](/CAS/20180808/GIF/63514-63-6.gif)
63514-63-6
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Yield:81937-39-5 121 g
Reaction Conditions:
with potassium tert-butylate in N,N-dimethyl acetamide at 70 - 75;Reagent/catalyst;Temperature;
Steps:
1.ii
100 g of compound I,35 g of potassium tert-butoxide,120g malonic acid diethyl ester was added to the DMA solution with stirring,Keep the reaction temperature 70 ° C ~ 75 ° C to TLC tracking of raw materials disappear.After the reaction is completed,The system is slowly poured into 1L ice water to quench,Stirring until solid precipitation,Filtered and dried to give Compound Π 121 g, a purity of 95%
References:
CN107522663,2017,A Location in patent:Paragraph 0024; 0031; 0038
81112-08-5
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105-53-3
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81937-39-5
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$51.00/250mg
103-84-4
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81937-39-5
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$51.00/250mg
![N-[4-(1-oxopropyl)phenyl]acetamide](/CAS/GIF/16960-49-9.gif)
16960-49-9
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81937-39-5
44 suppliers
$51.00/250mg