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7-Amino-5-chloroquinolin-8-ol → Quazolast

HRID 255495
ノート
印刷プレビュー

反応式

HRID 255495 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]([NH2:12])[C:9]([OH:13])=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2.[CH3:14][O:15][C:16](OC)([O:21]C)[C:17](OC)=O>>[C:16]([C:17]1[O:13][C:9]2[C:8]3[N:7]=[CH:6][CH:5]=[CH:4][C:3]=3[C:2]([Cl:1])=[CH:11][C:10]=2[N:12]=1)([O:15][CH3:14])=[O:21]
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

3

反応物 2

HCID 4174907-Amino-5-chloroquinolin-8-olHCID 12586559Methyl 2,2,2-trimethoxyacetate

生成物 1

HCID 24747Quazolast収率 51%

反応条件

温度
100 °C

実験手順

A mixture of 5-chloro-7-amino-8-hydroxyquinoline (6 g, 30.8 mol) and methyl trimethoxyacetate (16.3 g, 123.2 mol) was heated at 100° C. overnight. The reaction was cooled in an ice bath and filtered. The precipitate was dissolved in acetone (250 ml). The resulting solution was treated with charcoal at reflux, filtered through a pad of silica gel and celite and partially concentrated. Crystals formed which were filtered and dried giving 4.1 g (51% yield) of solid. M.P. 217°-218° C.

後処理

  1. temperatureThe reaction was cooled in an ice bath
  2. filtration
このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート
filtered
  • dissolutionThe precipitate was dissolved in acetone (250 ml)
  • additionThe resulting solution was treated with charcoal
  • temperatureat reflux
  • filtrationfiltered through a pad of silica gel and celite
  • concentrationpartially concentrated
  • customCrystals formed which
  • filtrationwere filtered
  • customdried
  • 出典と根拠

    ORDレコード
    ord-2f4df049dc904402b1cfac603896c91e
    出典データセット
    uspto-grants-1987_10
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04698346

    反応ノート

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