Reaktion #689420

Reaktionsgleichung

triethylamine

ethyl 2,2-difluoro-3-hydroxypentanoate

chloroform

methacrylic chloride

→

1-ethoxycarbonyl-1,1-difluoro-2-butyl methacrylate

Ausbeute 66.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionfollowed by extraction with chloroform one time
2. 2
   WaschenThe obtained organic layer was washed with diluted hydrochloric acid and water
3. 3
   Sonstigeby removing water with magnesium sulfate
4. 4
   Filtrationfiltration, chloroform
5. 5
   workup.DISTILLATIONwas distilled off

Vorschrift

A 25 ml reactor was charged with 1.50 g (8.2 mmol) of ethyl 2,2-difluoro-3-hydroxypentanoate, 6.5 g of chloroform, 10 mg of an antioxidant NONFLEX MBP made by Seiko Chemical Co., Ltd., 1.03 g (9.9 mmol, 1.2 eq) of methacrylic chloride, and 1.25 g (12.4 mmol, 1.5 eq) of triethylamine, followed by stirring at 55° C. for 4 hours. Then, 10 g of water was added, followed by extraction with chloroform one time. The obtained organic layer was washed with diluted hydrochloric acid and water, followed by removing water with magnesium sulfate. After conducting filtration, chloroform was distilled off, thereby obtaining 2.06 g of the target 1-ethoxycarbonyl-1,1-difluoro-2-butyl methacrylate. Purity was 66%, and yield was 66%.

Quelle