Dichloromethane → 4-(Benzyloxy)-2-fluorobenzonitrile

HRID 1456360노트

반응식

HRID 1456360 반응식
[CH2:1](Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[F:15][C:16]1[CH:23]=[C:22]([OH:24])[CH:21]=[CH:20][C:17]=1[C:18]#[N:19].ClCCl>C(#N)C>[F:15][C:16]1[CH:23]=[C:22]([O:24][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:21]=[CH:20][C:17]=1[C:18]#[N:19]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 27346752-Fluoro-4-hydroxybenzonitrile

생성물 1

HCID 113336284-(Benzyloxy)-2-fluorobenzonitrile수율 84.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

15.2 ml (0.127 mol) of benzyl bromide and 29.3 g (0.212 mol) of potassium carbonate are added to a solution of 13.3 g (0.106 mol) of 2-fluoro-4-hydroxybenzonitrile in 150 ml of acetonitrile. The mixture is stirred at reflux for 1 hour 30 minutes and then filtered, the filtrate is concentrated under reduced pressure, and the oil obtained is diluted in the minimum amount of dichloromethane. After crystallization by addition of diisopropyl ether, filtration and drying, 20.3 g of product are obtained. Melting point : 87° C.

후처리

  1. temperatureat reflux for 1 hour 30 minutes
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customthe oil obtained
  5. customAfter crystallization
  6. additionby addition of diisopropyl ether, filtration
  7. customdrying

출처 및 근거

ORD 기록
ord-896ec0e06715400fa274248c5d1f7a22
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05843975

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