1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 13071762、化合物

HRID 2418470ノート

反応式

HRID 2418470 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][C:11]([Cl:18])=[C:12]([F:17])[CH:13]=2)[N:8]([CH2:19][CH2:20]Cl)[CH:7]=1)=[O:5])[CH3:2].C1CCN2C(=NCCC2)CC1>CS(C)=O>[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][C:11]([Cl:18])=[C:12]([F:17])[CH:13]=2)[N:8]([CH:19]=[CH2:20])[CH:7]=1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 6212337-Chloro-1-(2-chloroethyl)-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid, ethyl ester

生成物 1

HCID 13071762HCID 13071762、化合物収率 65.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a 120 ml of anhydrous dimethyl sulfoxide (DMSO), 6.32 g of 1-(2-chloroethyl)-6-fluoro-7-chloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester and 2.89 g of 1,8-diazabicyclo[5,4,0]-7-undecene were added and the mixture was heated at 84°-89° C. for 2 hrs. The reaction mixture was concentrated in vacuo and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried. The residue obtained through evaporation of chloroform was recrystallized from ethyl ether to give 3.66 g (65.1% yield) of 1-vinyl-6-fluoro-7-chloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester. mp: 146°-149° C.

後処理

  1. temperaturethe mixture was heated at 84°-89° C. for 2 hrs
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionthe residue was dissolved in chloroform
  4. washThe chloroform layer was washed with water
  5. customdried
  6. customThe residue obtained through evaporation of chloroform
  7. customwas recrystallized from ethyl ether

出典と根拠

ORDレコード
ord-1532107dbffa44fda9a11e8418d196ea
出典データセット
uspto-grants-1984_09
特許番号
US04472579

反応ノート

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