Hydrochloric Acid → HCID 13627533、化合物

HRID 1589617ノート

反応式

HRID 1589617 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(=O)([O-])[O-].[Ca+2].Cl>C1C=CC=CC=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:18])[C:15]([CH3:17])=[CH2:16]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 13528Methacryloyl chlorideHCID 3613333Benzonitrile, 2,3,5,6-tetrafluoro-4-hydroxy-

生成物 1

HCID 13627533HCID 13627533、化合物収率 63.9%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

In 30 ml of benzene, 3.0 g (0.0157 mol) of 4-cyano-2,3,5,6-tetrafluorophenol and 1.80 g (0.0173 mol) of methacrylic acid chloride were dissolved. The resultant solution, and 1.73 g (0.0173 mol) of calcium carbonate added thereto as a hydrogen chloride trapping agent were stirred under reflux for 32 hours. The resultant reaction mixture was cooled off and filtered to separate calcium carbonate. The filtrate was dried with magnesium sulfate and then evaporated with a rotary evaporator. Consequently, there was obtained 2.6 g of 4-cyano-2,3,5,6-tetrafluorophenyl methacrylate (yeild 63.9% and purity 95.4%). The analyses obtained of the novel substance for the determination of its chemical structure were the same as those of Example 2.

後処理

  1. temperatureunder reflux for 32 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 with a rotary evaporator

出典と根拠

ORDレコード
ord-bb95f3264134436e971880920d32f9bb
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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