Chloroform → 1-Ethoxycarbonyl-1,1-difluoro-2-butyl methacrylate

HRID 1929271노트

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HRID 1929271 반응식
[F:1][C:2]([F:12])([CH:8]([OH:11])[CH2:9][CH3:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4].C(Cl)(Cl)Cl.[C:17](Cl)(=[O:21])[C:18]([CH3:20])=[CH2:19].C(N(CC)CC)C>O>[C:17]([O:11][CH:8]([CH2:9][CH3:10])[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])([F:12])[F:1])(=[O:21])[C:18]([CH3:20])=[CH2:19]

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 59863825Ethyl 2,2-difluoro-3-hydroxypentanoate

생성물 1

HCID 598638611-Ethoxycarbonyl-1,1-difluoro-2-butyl methacrylate수율 66%

시약·촉매·용매 1

HCID 962Water용매

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온도
55 °C

실험 절차

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%.

후처리

  1. extractionfollowed by extraction with chloroform one time
  2. washThe obtained organic layer was washed with diluted hydrochloric acid and water
  3. customby removing water with magnesium sulfate
  4. filtrationfiltration, chloroform
  5. distillationwas distilled off

출처 및 근거

ORD 기록
ord-edaaee7bd7544bc391c5648b672f0849
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08187787B2

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