Toluene → 2-(3-Hydroxyphenoxy)-6-(trifluoromethyl)benzonitrile

HRID 354094노트

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HRID 354094 반응식
[C:1]1([CH:8]=[CH:7][CH:6]=[C:4]([OH:5])[CH:3]=1)[OH:2].[OH-].[K+].Cl[C:12]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[C:13]=1[C:14]#[N:15].C1(C)C=CC=CC=1>CN1CCCC1=O.O>[C:14]([C:13]1[C:16]([C:20]([F:21])([F:22])[F:23])=[CH:17][CH:18]=[CH:19][C:12]=1[O:2][C:1]1[CH:8]=[CH:7][CH:6]=[C:4]([OH:5])[CH:3]=1)#[N:15]

참가 물질

7

반응물 4

HCID 1140TolueneHCID 5054ResorcinolHCID 14797Potassium HydroxideHCID 108674572-Chloro-6-(trifluoromethyl)benzonitrile

생성물 1

HCID 129718822-(3-Hydroxyphenoxy)-6-(trifluoromethyl)benzonitrile

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

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온도
62.5 °C

실험 절차

Resorcinol [44.0 g (0.4 mol)] is partly dissolved in 170 ml of N-methylpyrrolidone, and potassium hydroxide [min. 85% pure; 34.5 g (0.52 mol)] and then 2-chloro-6-(trifluoromethyl)benzonitrile [20.5 g (0.1 mol)] are added. The mixture is stirred at 60-65° C. for 2.5 h. After addition of 300 ml of toluene and 400 ml of water, the aqueous phase is separated off and extracted once more with 300 ml of toluene. The combined organic phases are dried over MgSO4 and, after filtration, concentrated. Digestion of the oily residue with 150 ml of water, filtration and drying affords pale brownish crystals.

후처리

  1. customthe aqueous phase is separated off
  2. extractionextracted once more with 300 ml of toluene
  3. dry with materialThe combined organic phases are dried over MgSO4
  4. filtrationafter filtration
  5. concentrationconcentrated
  6. filtrationDigestion of the oily residue with 150 ml of water, filtration
  7. customdrying
  8. customaffords pale brownish crystals

출처 및 근거

ORD 기록
ord-2945f618b9dd40b1844272a909f19fa1
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756409B2

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