Allyl methacrylate → 2-(7-Methoxynaphthalen-1-yl)acetonitrile

HRID 1297553

반응식

HRID 1297553 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH:9]=[C:10]2[CH2:13][C:14]#[N:15])=[CH:5][CH:4]=1.C(OCC=C)(=O)C(C)=C>C1(C)C=CC=CC=1.[Pd]>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[CH:8][CH:9]=[C:10]2[CH2:13][C:14]#[N:15])=[CH:5][CH:4]=1

참가 물질

5

반응물 2

HCID 7274Allyl methacrylateHCID 11287102(7-Methoxy-3,4-dihydronaphthalen-1-yl)acetonitrile

생성물 1

HCID 112640682-(7-Methoxynaphthalen-1-yl)acetonitrile수율 91%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 1140Toluene용매2회

실험 절차

There are introduced into a 670 litre reactor 12.6 kg of 5% palladium-on-carbon in toluene, which is heated at reflux; then 96.1 kg of (7-methoxy-3,4-dihydro-1-naphthalenyl)-acetonitrile dissolved in toluene are added as well as 63.7 kg of allyl methacrylate. The reaction is continued at reflux and is followed by vapour phase chromatography. When all the starting substrate has disappeared, the reaction mixture is cooled to ambient temperature and then filtered. After removal of the toluene by evaporation, the resulting solid residue is recrystallised from an ethanol/water (80/20) mixture to give the title product in a yield of 91% and with a chemical purity exceeding 99%.

후처리

  1. temperatureis heated
  2. temperatureat reflux
  3. temperatureat reflux
  4. filtrationfiltered
  5. customAfter removal of the toluene
  6. customby evaporation
  7. customthe resulting solid residue is recrystallised from an ethanol/water (80/20) mixture

출처 및 근거

ORD 기록
ord-e135be7e7c264e28ad1f527541d77f90
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07250531B2

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