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

Hydrochloric Acid → 7-bromo-9h-fluoren-2-ol

HRID 2416353
ノート
印刷プレビュー

反応式

HRID 2416353 の反応式
[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([O:15]C(=O)C)=[CH:9][CH:10]=3)[CH2:5][C:4]=2[CH:3]=1.[OH-].[Li+].Cl>C(O)CO>[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([OH:15])=[CH:9][CH:10]=3)[CH2:5][C:4]=2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 22630262HCID 22630262、化合物

生成物 1

HCID 2635827-bromo-9h-fluoren-2-ol収率 67.3%

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

A mixture of 2-bromo-7-acetoxyfluorene (69 g), lithium hydroxide (9 g) and ethylene glycol (350 mL) was heated for one hour while refluxing. The reaction mixture was poured into 6M-hydrochloric acid (300 mL) to terminate the reaction, and the product was extracted with ethyl acetate (350 mL). The ethyl acetate layer was washed with a saturated sodium carbonate aqueous solution and dried on anhydrous magnesium sulfate. A residue obtained by distilling the solvent off under reduced pressure was recrystallized from chloroform to obtain 2-bromo-7-hydroxyfluorene (40 g) of colorless needle crystal. The melting point was 183-184° C.

後処理

  1. temperaturewas heated for one hour
  2. temperaturewhile refluxing
  3. customto terminate
  4. customthe reaction
  5. extractionthe product was extracted with ethyl acetate (350 mL)
  6. washThe ethyl acetate layer was washed with a saturated sodium carbonate aqueous solution
  7. dry with materialdried on anhydrous magnesium sulfate
  8. customA residue obtained
  9. distillationby distilling the solvent off under reduced pressure
  10. customwas recrystallized from chloroform

出典と根拠

ORDレコード
ord-2fa3b35cd4c54afcbe64b218d958f629
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06824709B2

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