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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
ノート
印刷プレビュー

反応式

HRID 2377795 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
235 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7113174d69b9471faa06ebc43083603d
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07470708B2

反応ノート

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