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ChemicalBook CAS DataBase List Cyclopropyl 2-fluorobenzyl ketone

Cyclopropyl 2-fluorobenzyl ketone synthesis

14synthesis methods
-

Yield:150322-73-9 96 %

Reaction Conditions:

with nickel(II) bromide dimethoxyethane;TBADT;sodium carbonate;4,4'-di-tert-butyl-2,2'-bipyridine in acetone at 35;Inert atmosphere;Sealed tube;Sonication;

Steps:

1 Example 1

A magnetic stirring bar was added to the dry reaction flask, filled with argon protection, and 4,4'-di-tert-butyl-2,2'-dipyridine (0.002mol, 0.54g), nickel bromide ethylene glycol dihydrate were added in turn Methyl ether complex (0.002mol, 0.62g), add 100mL of acetone to dissolve, ultrasonicate until the solution is homogeneous, then add sodium carbonate (0.06mol, 6.36g), tetrabutylammonium decapolytungstic acid to the reaction flask in turn Salt (0.0004mol, 1.328g), 1-bromomethyl-2-fluorobenzene (0.02mol, 3.76g), cyclopropylcarbaldehyde (0.03mol, 2.10g), filled with argon protection. After sealing, light was illuminated under a 390-nanometer light source, the light source was about 6 cm away from the reaction flask, the fan was cooled, and the temperature was controlled to 35 ° C. After 3 hours, 100 mL of acetone was added to dilute, concentrated under reduced pressure, and directly separated and purified by column chromatography (n-hexane:acetic acid). ethyl ester=19:1) to obtain 3.42 g of the prasugrel intermediate of formula I.

References:

CN114874061,2022,A Location in patent:Paragraph 0057-0060; 0082

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