Acryloyl chloride → HCID 13627534、化合物

HRID 1589618ノート

反応式

HRID 1589618 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:17])[CH:15]=[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:17])[CH:15]=[CH2:16]

参加物

4

反応物 2

HCID 13140Acryloyl chlorideHCID 3613333Benzonitrile, 2,3,5,6-tetrafluoro-4-hydroxy-

生成物 1

HCID 13627534HCID 13627534、化合物収率 62%

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 11.3 g (0.125 mol) of acrylic acid chloride were dissolved. To the resultant solution, 20 g of molecular sieve 3 Å in diameter was added. The mixture was stirred under reflux for 38 hours. The resultant reaction mixture was cooled off and filtered to separate the molecular sieve. The filtrate was dried with magnesium sulfate and evaporated to dryness with a rotary evaporator. Consequently, there was obtained 15.2 g of 4-cyano-2,3,5,6-tetrafluorophenyl acrylate (yield 62.0% based on 4-cyano-2,3,5,6-tetrafluorophenol, purity 96.4%) having a melting point below determined.

後処理

  1. temperatureunder reflux for 38 hours
  2. customThe resultant reaction mixture
  3. temperaturewas cooled off
  4. filtrationfiltered
  5. customto separate the molecular sieve
  6. dry with materialThe filtrate was dried with magnesium sulfate
  7. customevaporated to dryness with a rotary evaporator

出典と根拠

ORDレコード
ord-30b0eae3a0dd4aa8a2648f9d5e342602
出典データセット
uspto-grants-1986_02
特許番号
US04572805

反応ノート

読み込み中…