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ChemicalBook CAS DataBase List Hexamethylene diacrylate
13048-33-4

Hexamethylene diacrylate synthesis

5synthesis methods
-

Yield:13048-33-4 99%

Reaction Conditions:

with 4-acetylamino-2,2,6,6-tetramethylpiperidine-1-oxyl;(4,4'-dimethyl-1,1'-biphenyl);bis(2,6-t-butyl-4-methylphenoxo)magnesium at 25; for 0.5 h;Molecular sieve;

Steps:

28 Manufacturing of carboxylic acid ester

General procedure: In a flask, 400 mg of dried molecular sieve 5 ?, 24.2 mg (0.1 mmol) of NaOAr-1, methyl methacrylate (hereinafter, may be abbreviated as “MMA”) 1.49 mL (room temperature (25 ° C.)) (14 mmol), 4-Acetylamino-2,2,6,6-tetramethylpiperidin-1-oxyl 4.3 mg (0.1 mmol) as a polymerization inhibitor And 4,4'-dimethylbiphenyl 36.5 mg (0.2 mmol) was added as an internal standard substance, and the mixture was stirred at room temperature (25 ° C.) for 3 minutes, and then. Benzyl alcohol (hereinafter, also abbreviated as "BnOH") 0.206 mL (2 mmol) was added to obtain a suspension. The suspension was then stirred at room temperature (25 ° C.) for 30 minutes. When a part of the suspension was sampled and the yield was determined by 1H-NMR (CDCl3), it exceeded 99%. The sample used for obtaining the yield was returned to the suspension, and the obtained suspension was purified as it was on a silica gel column (mobile phase: hexane / methyl acetate) to obtain the compound of Example 1.

References:

JP2021/137728,2021,A Location in patent:Paragraph 0105-0109; 0160-0161; 0180-0181

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