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

2',4'-Dihydroxyacetophenone → 1-(2-Hydroxy-4-(methoxymethoxy)phenyl)ethanone

HRID 1879552
ノート
印刷プレビュー

反応式

HRID 1879552 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[C:9](=[O:11])[CH3:10].C([O-])([O-])=O.[K+].[K+].Cl[CH2:19][O:20][CH3:21]>CC(C)=O>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH2:19][O:20][CH3:21])[CH:5]=[CH:4][C:3]=1[C:9](=[O:11])[CH3:10]
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 69902',4'-DihydroxyacetophenoneHCID 7864Chloromethyl Methyl EtherHCID 11430Potassium Carbonate

生成物 1

HCID 117455591-(2-Hydroxy-4-(methoxymethoxy)phenyl)ethanone収率 61.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To 1-(2,4-dihydroxyphenyl)ethanone (1.52 g, 10 mmol) in 12 mL acetone was added K2CO3 (1.38 g, 10 mmol) followed by slow addition of chloro(methoxy)methane (885 mg, 11 mmol) with stirring under Ar atmosphere at rt. The reaction mixture was stirred at rt for 4 h and filtered. Solid was washed with EtOAc (80 mL) and the combined filtrate was washed with NaH2PO4 (sat. 50 mL) and water (80 mL) and dried over MgSO4 and concentrated. The crude product was purified with silica chromatography (hexane/EtOAc) to afford 1-(2-hydroxy-4-(methoxymethoxy)phenyl)ethanone as a off-white solid (1.2 g, 61%). MS (ESI) m/z 197 (M+H+).

後処理

  1. stirringThe reaction mixture was stirred at rt for 4 h
  2. filtrationfiltered
  3. washSolid was washed with EtOAc (80 mL)
  4. washthe combined filtrate was washed with NaH2PO4 (sat. 50 mL) and water (80 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. customThe crude product was purified with silica chromatography (hexane/EtOAc)

出典と根拠

ORDレコード
ord-aba515d1a6f74cd1ba57b962ba9da9eb
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318132B2

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