Water → HCID 22227324、化合物

HRID 2395807ノート

反応式

HRID 2395807 の反応式
Br[C:2]([F:16])([F:15])[C:3](F)([F:13])[O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[O:10])=[CH:7][CH:6]=1.O>[Zn].C(#N)C>[F:13][C:3]([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[O:10])=[CH:7][CH:6]=1)=[C:2]([F:16])[F:15]

参加物

5

反応物 2

HCID 962WaterHCID 18990557HCID 18990557、化合物

生成物 1

HCID 22227324HCID 22227324、化合物収率 63.3%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 6342Acetonitrile溶媒

反応条件

温度
79 °C

実験手順

Acetonitrile (300 ml) and granular zinc (30.0 g) are combined in a 1 liter round bottomed flask and stirred at 75° C. under nitrogen as 4-(2-bromotetrafluoroethoxy)benzaldehyde (111.39 g, 0.37 mole) is added slowly by dropping addition funnel. The resulting mixture is stirred and heated at 79° C. for 12 hours. After filtration to remove zinc salts and unreacted zinc, the acetonitrile is removed under vacuum on a rotary evaporator. The resulting oily residue is flash distilled on a rotary evaporator under high vacuum (26.6 Pa) to provide 47.33 g (0.234 mole) of a water white oil in 63.3 percent yield.

後処理

  1. additionis added slowly
  2. additionaddition funnel
  3. filtrationAfter filtration
  4. customto remove zinc salts and unreacted zinc
  5. customthe acetonitrile is removed under vacuum on a rotary evaporator
  6. distillationdistilled on a rotary evaporator under high vacuum (26.6 Pa)

出典と根拠

ORDレコード
ord-cdefe62b020d4375861ab2730fd1eb2d
出典データセット
uspto-grants-1996_02
特許番号
US05489623

反応ノート

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