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Sodium Bicarbonate → 4-Chloroquinolin-7-ol

HRID 1791569
ノート
印刷プレビュー

反応式

HRID 1791569 の反応式
C([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13]([Cl:19])=[CH:14][CH:15]=[N:16]2)=[CH:11][CH:10]=1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>C(O)(C(F)(F)F)=O>[Cl:19][C:13]1[C:12]2[C:17](=[CH:18][C:9]([OH:8])=[CH:10][CH:11]=2)[N:16]=[CH:15][CH:14]=1
参加物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 516892Sodium BicarbonateHCID 220306577-(Benzyloxy)-4-chloroquinoline

生成物 1

HCID 1357290834-Chloroquinolin-7-ol収率 98%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 7-benzyloxy-4-chloroquinoline (17 g, 56 mmol), (Konishi et al. WO 96/11187), in TFA (170 ml) was heated at reflux for 2 hours. The solvent was removed under vacuum and the residue was triturated with ether, filtered and washed with ether. The solid was suspended in an aqueous solution of sodium hydrogen carbonate (5.5 g, 65 mmol in 200 ml of water) and stirred at ambient temperature for 30 minutes. The solid was collected by filtration, washed with water and dried overnight under vacuum and over phosphorus pentoxide to give 4-chloro-7-hydroxyquinoline (9.85 g, 98%).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureat reflux for 2 hours
  2. customThe solvent was removed under vacuum
  3. customthe residue was triturated with ether
  4. filtrationfiltered
  5. washwashed with ether
  6. filtrationThe solid was collected by filtration
  7. washwashed with water
  8. dry with materialdried overnight under vacuum and over phosphorus pentoxide

出典と根拠

ORDレコード
ord-d53e2547fb874bd493ae351e58fef713
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07074800B1

反応ノート

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