Benzene → HCID 13627534、化合物

HRID 1589619ノート

反応式

HRID 1589619 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](=[O:17])([O-])[O-].[Ca+2].Cl.[CH:20]1C=CC=C[CH:21]=1>>[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:20]=[CH2:21]

参加物

5

反応物 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 3613333Benzonitrile, 2,3,5,6-tetrafluoro-4-hydroxy-

生成物 1

HCID 13627534HCID 13627534、化合物収率 57.1%

実験手順

In 30 ml of benzene, 3.82 g (0.020 mol) of 4-cyano-2,3,5,6-tetrafluorophenol and 2.26 g (0.025 mol) of calcium carbonate added thereto as a hydrogen chloride trapping agent were stirred under reflux for 40 hours. The resultant reaction mixture was cooled off and filtered to separate calcium carbonate. The filtrate was dried with magnesium sulfate and then evaporated to dryness with a rotary evaporator. Consequently, there was obtained 2.8 g of 4-cyano-2,3, 5,6-tetrafluorophenyl acrylate (yield 57.1%, purity 95.8%). The analyses obtained of the novel substance for the determination of its chemical structure were the same as those of Example 5.

後処理

  1. temperatureunder reflux for 40 hours
  2. customThe resultant reaction mixture
  3. temperaturewas cooled off
  4. filtrationfiltered
  5. customto separate calcium carbonate
  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-1cac325459d943e8af594be5dcaab32f
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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