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

HRID 1363908노트

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HRID 1363908 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-2bdfb55318ab4c9cb9f22bd3ba5c9aa0
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07887990B2

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