Triethylamine → 1-Ethyl-4-(trifluoromethyl)cyclohexyl methacrylate

HRID 41846

反応式

HRID 41846 の反応式
[CH2:1]([C:3]1([OH:13])[CH2:8][CH2:7][CH:6]([C:9]([F:12])([F:11])[F:10])[CH2:5][CH2:4]1)[CH3:2].C(N(CC)CC)C.[C:21](Cl)(=[O:25])[C:22]([CH3:24])=[CH2:23]>CN(C)C1C=CN=CC=1.CC(C)=O>[C:21]([O:13][C:3]1([CH2:1][CH3:2])[CH2:4][CH2:5][CH:6]([C:9]([F:10])([F:12])[F:11])[CH2:7][CH2:8]1)(=[O:25])[C:22]([CH3:24])=[CH2:23]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 647565111-Ethyl-4-trifluoromethylcyclohexanol

生成物 1

HCID 679692611-Ethyl-4-(trifluoromethyl)cyclohexyl methacrylate収率 75.7%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 180Acetone溶媒2 回

実験手順

A four-necked flask equipped with a stirrer, a thermometer, and a dropping funnel was charged with 7.9 g (0.04 mol) of 1-ethyl-4-trifluoromethylcyclohexanol, 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 8.0 g of 1-ethyl-4-(trifluoromethyl)cyclohexyl methacrylate (hereinafter may be referred to as “compound (M-3)” ((M-3) in Table 1)). The yield of 1-ethyl-4-(trifluoromethyl)cyclohexyl methacrylate with respect to 1-ethyl-4-trifluoromethylcyclohexanol was 76%.

後処理

  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

出典と根拠

ORDレコード
ord-d932d86fdda44311868fb1815d018b40
出典データセット
uspto-grants-2013_09
特許番号
US08535871B2

関連ノート

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