Formic Acid → 5-Bromo-2-nitrothiophene-3-carbaldehyde

HRID 1967146

反応式

HRID 1967146 の反応式
[Br:1][C:2]1[S:6][C:5]([N+:7]([O-:9])=[O:8])=[C:4]([CH:10](Cl)Cl)[CH:3]=1.C(O)=[O:14]>[Cl-].[Zn+2].[Cl-].O>[Br:1][C:2]1[S:6][C:5]([N+:7]([O-:9])=[O:8])=[C:4]([CH:10]=[O:14])[CH:3]=1

参加物

5

反応物 2

HCID 284Formic AcidHCID 595256075-Bromo-3-(dichloromethyl)-2-nitrothiophene

生成物 1

HCID 534029475-Bromo-2-nitrothiophene-3-carbaldehyde

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 962Water溶媒

実験手順

5-Bromo-3-(dichloromethyl)-2-nitrothiophene (60.5 g, 208 mmol) and zinc chloride (113 g, 832 mmol) were stirred in refluxing formic acid (800 mL) overnight. After cooling to ambient temperature, water was added and the mixture was extracted with EtOAc (4×). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo to give the title compound as an orange solid.

後処理

  1. extractionthe mixture was extracted with EtOAc (4×)
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f68080b21a334d46956aa02fd6a2cd4c
出典データセット
uspto-grants-2013_04
特許番号
US08420695B2

関連ノート

読み込み中…