Methacryloyl chloride → HCID 13627533、化合物

HRID 1589615ノート

反応式

HRID 1589615 の反応式
[C:1]([C:3]1[C:8]([F:9])=[C:7]([F:10])[C:6]([OH:11])=[C:5]([F:12])[C:4]=1[F:13])#[N:2].[C:14](Cl)(=[O:18])[C:15]([CH3:17])=[CH2:16]>C(Cl)(Cl)(Cl)Cl>[C:14]([O:11][C:6]1[C:5]([F:12])=[C:4]([F:13])[C:3]([C:1]#[N:2])=[C:8]([F:9])[C:7]=1[F:10])(=[O:18])[C:15]([CH3:17])=[CH2:16]

参加物

4

反応物 2

HCID 13528Methacryloyl chlorideHCID 3613333Benzonitrile, 2,3,5,6-tetrafluoro-4-hydroxy-

生成物 1

HCID 13627533HCID 13627533、化合物収率 83.8%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

In 200 ml of carbon tetrachloride, 19.1 g (0.100 mol) of 4-cyano-2,3,5,6-tetrafluorophenol and 13.0 g (0.125 mol) of methacrylic acid chloride were dissolved. To the resultant solution was added 20 g of molecular sieve 3 Å in diameter. The resultant mixture was refluxed as agitated for 48 hours. The reaction mixture so produced was cooled and then filtered to separate the molecular sieve. The filtrate was dried with magnesium sulfate and then evaporated to dryness with a rotary evaporator. Consequently, there was obtained 21.7 g of 4-cyano-2,3,5,6-tetrafluorophenyl methacrylate (yield 83.8% based on 4-cyano-2,3,5,6-tetrafluorophenol, purity 96.5%).

後処理

  1. customThe reaction mixture so produced
  2. temperaturewas cooled
  3. filtrationfiltered
  4. customto separate the molecular sieve
  5. dry with materialThe filtrate was dried with magnesium sulfate
  6. customevaporated to dryness with a rotary evaporator

出典と根拠

ORDレコード
ord-f5d1d169c0c448b887376a42aed92100
出典データセット
uspto-grants-1986_02
特許番号
US04572805

反応ノート

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