ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Diethyl Ether → 3-(Benzyloxy)-2-hydroxybenzaldehyde

HRID 253449
ノート
印刷プレビュー

反応式

HRID 253449 の反応式
[Mg].CCOCC.BrBr.C([O:16][C:17]1[C:24]([O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[CH:23][CH:22]=[CH:21][C:18]=1[CH:19]=[O:20])C1C=CC=CC=1>C1C=CC=CC=1>[CH2:26]([O:25][C:24]1[C:17]([OH:16])=[C:18]([CH:21]=[CH:22][CH:23]=1)[CH:19]=[O:20])[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 24408Bromine2 回HCID 5462224MagnesiumHCID 10870855Dibenzyloxybenzaldehyde

生成物 1

HCID 112876163-(Benzyloxy)-2-hydroxybenzaldehyde

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To magnesium (2.9 g, turnings, 0.12 mol) in a mixture of anhydrous ether (85 mL) and benzene (85 mL) at 0° C., bromine (3.4 mL, 0.066 mol) was added dropwise. When the reaction had started, stirring was commenced and the addition of bromine continued until complete. The ice bath was removed and the reaction mixture was heated until the solution was almost colorless. After cooling down, the reaction mixture was slowly added to a solution of 2,3-bis-benzyloxy-benzaldehyde (128, 20 g, 0.063 mol) in benzene (415 mL) at room temperature while stirring vigorously. Upon completion of the addition, the reaction mixture was stirred at room temperature overnight, and then refluxed for 36 hours. After the reaction mixture was cooled down to room temperature, a solid was collected by filtration and washed with benzene, then boiled in hydrochloric acid (100 mL, 1.0 M) for 30 minutes. After cool down, the solution was extracted with dichloromethane. The organic layer was washed with brine and dried over magnesium sulfate. A light tan solid was obtained after removal of the solvent (129, 12.5 g, 87%).

後処理

  1. customThe ice bath was removed
  2. temperaturethe reaction mixture was heated until the solution
  3. temperatureAfter cooling down
  4. stirringwhile stirring vigorously
  5. additionUpon completion of the addition
  6. stirringthe reaction mixture was stirred at room temperature overnight
  7. temperaturerefluxed for 36 hours
  8. filtrationa solid was collected by filtration
  9. washwashed with benzene
  10. temperatureAfter cool down
  11. extractionthe solution was extracted with dichloromethane
  12. washThe organic layer was washed with brine
  13. dry with materialdried over magnesium sulfate
  14. customA light tan solid was obtained
  15. customafter removal of the solvent (129, 12.5 g, 87%)

出典と根拠

ORDレコード
ord-a636ba893aca4f16a6a79a1cb4eaebb5
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07872018B2

反応ノート

読み込み中…

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