Acryloyl chloride → HCID 13627534, 화합물

HRID 1589618노트

반응식

HRID 1589618 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 13627534HCID 13627534, 화합물수율 62%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-30b0eae3a0dd4aa8a2648f9d5e342602
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04572805

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