Water → HCID 22227324, 화합물

HRID 21998노트

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HRID 21998 반응식
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]

참가 물질

5

반응물 2

HCID 962WaterHCID 18990557HCID 18990557, 화합물

생성물 1

HCID 22227324HCID 22227324, 화합물수율 63.3%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 6342Acetonitrile용매

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온도
79 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d32ce7e50ce74a6abd953f8a517f7829
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05426164

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