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1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → Methyl 6-fluoro-4-oxo-1,4-dihydroquinoline-2-carboxylate

HRID 2377795
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인쇄 미리보기

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HRID 2377795 반응식
C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.[CH3:26][O:27][C:28](=[O:43])[C:29]([NH:35][C:36]1[CH:41]=[CH:40][C:39]([F:42])=[CH:38][CH:37]=1)=[CH:30][C:31]([O:33]C)=O>CO>[F:42][C:39]1[CH:38]=[C:37]2[C:36](=[CH:41][CH:40]=1)[NH:35][C:29]([C:28]([O:27][CH3:26])=[O:43])=[CH:30][C:31]2=[O:33]
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참가 물질

4

반응물 2

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)HCID 691174942-(4-Fluorophenylamino)but-2-enedioic Acid Dimethyl Ester

생성물 1

HCID 11390401Methyl 6-fluoro-4-oxo-1,4-dihydroquinoline-2-carboxylate

시약·촉매·용매 1

HCID 887Methanol용매

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온도
235 °C

실험 절차

250 ml de Dowtherm-A are brought to reflux (about 235° C.) under a nitrogen atmosphere. 41 g (0.16 M) of 2-(4-fluorophenylamino)but-2-enedioic acid dimethyl ester are then introduced dropwise. The methanol formed is separated out. Refluxing is maintained for 10 minutes after the end of introduction. The reaction mixture is then cooled to about 50° C., followed by addition of 250 ml of petroleum ether: a solid precipitates out. It is filtered off by suction, washed three times with petroleum ether and then dried under reduced pressure.

후처리

  1. customis separated out
  2. temperatureRefluxing
  3. temperatureis maintained for 10 minutes after the end of introduction
  4. temperatureThe reaction mixture is then cooled to about 50° C.
  5. additionfollowed by addition of 250 ml of petroleum ether
  6. customa solid precipitates out
  7. filtrationIt is filtered off by suction
  8. washwashed three times with petroleum ether
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-7113174d69b9471faa06ebc43083603d
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07470708B2

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