Ethanedioyl dibromide → 4-Bromo-5,5-dimethylfuran-2-one

HRID 383484

反応式

HRID 383484 の反応式
O[C:2]1[C:6]([CH3:8])([CH3:7])[O:5][C:4](=[O:9])[CH:3]=1.C(Br)(=O)C([Br:13])=O>ClCCCl.CN(C=O)C>[Br:13][C:2]1[C:6]([CH3:8])([CH3:7])[O:5][C:4](=[O:9])[CH:3]=1

参加物

5

反応物 2

HCID 84841Ethanedioyl dibromideHCID 547201394-Hydroxy-5,5-dimethyl-2(5H)-furanone

生成物 1

HCID 126719604-Bromo-5,5-dimethylfuran-2-one収率 86.2%

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-hydroxy-5, 5-dimethyl-5H-furan-2-one (2.1 g, 16.4 mmol) in DCE (40 mL) and DMF (1.5 mL) at 0° C. was added dropwise oxalyl bromide (3.0 mL, 32 mmol, 2 equiv). The mixture was stirred at room temperature for 4-5 h, and then put in an ice bath. Ice water (100 mL) was added slowly. The mixture was extracted with CH2Cl2 (100 mL). The organic phase was washed with 10% NaHCO3 and again with water, dried over sodium sulfate and evaporated to give the title compound 2.7 g (86% yield).

後処理

  1. customput in an ice bath
  2. extractionThe mixture was extracted with CH2Cl2 (100 mL)
  3. washThe organic phase was washed with 10% NaHCO3 and again with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated

出典と根拠

ORDレコード
ord-260a2582978345039ad1ee6764745a2e
出典データセット
uspto-grants-2013_02
特許番号
US08367664B2

関連ノート

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