Triethylamine → 1-Ethyl-4,4-difluorocyclohexyl methacrylate

HRID 41848

반응식

HRID 41848 반응식
[CH2:1]([C:3]1([OH:11])[CH2:8][CH2:7][C:6]([F:10])([F:9])[CH2:5][CH2:4]1)[CH3:2].C(N(CC)CC)C.[C:19](Cl)(=[O:23])[C:20]([CH3:22])=[CH2:21]>CN(C)C1C=CN=CC=1.CC(C)=O>[C:19]([O:11][C:3]1([CH2:1][CH3:2])[CH2:4][CH2:5][C:6]([F:10])([F:9])[CH2:7][CH2:8]1)(=[O:23])[C:20]([CH3:22])=[CH2:21]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 666026041-Ethyl-4,4-difluorocyclohexanol

생성물 1

HCID 679692711-Ethyl-4,4-difluorocyclohexyl methacrylate수율 79.9%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 180Acetone용매2회

실험 절차

A four-necked flask equipped with a stirrer, a thermometer, and a dropping funnel was charged with 6.6 g (0.04 mol) of 1-ethyl-4,4-difluorocyclohexanol, 0.2 g of 4-dimethylaminopyridine, 4.9 g of triethylamine, and 20 g of acetone. The mixture was stirred to obtain a solution. A solution prepared by dissolving 4.6 g (0.044 mol) of methacrylic acid chloride in 5 g of acetone was added to the solution at 4° C. over 30 minutes. The mixture was stirred at 4° C. for 3 hours to obtain a reaction mixture. The reaction mixture was washed with water to obtain 7.42 g of 1-ethyl-4,4-difluorocyclohexyl methacrylate (hereinafter may be referred to as “compound (M-8)” ((M-8) in Table 1)). The yield of 1-ethyl-4,4-difluorocyclohexyl methacrylate with respect to 1-ethyl-4,4-difluorocyclohexanol was 78%.

후처리

  1. customA four-necked flask equipped with a stirrer
  2. customto obtain a solution
  3. customA solution prepared
  4. additionwas added to the solution at 4° C. over 30 minutes
  5. stirringThe mixture was stirred at 4° C. for 3 hours
  6. customto obtain a reaction mixture
  7. washThe reaction mixture was washed with water

출처 및 근거

ORD 기록
ord-ae4ed1cf31ce486a998b94fc968f4a3b
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08535871B2

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