Sodium Iodide → 84422-52-6

HRID 493208

反応式

HRID 493208 の反応式
C[O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([CH3:13])=[CH:7][C:4]=1[CH:5]=[O:6].[I-].[Na+].[Al+3].[Cl-].[Cl-].[Cl-]>C(#N)C>[OH:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([CH3:13])=[CH:7][C:4]=1[CH:5]=[O:6]

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 2516922,4-Dimethoxy-5-methylbenzaldehydeHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 1316681984422-52-6

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The above prepared 2,4-Dimethoxy-5-methyl-benzaldehyde (5.40 g, 30 mmol) was dissolved in 150 mL of acetonitrile and treated successively with sodium iodide (6.74 g, 1.5 eq.) and AlCl3 (4.00 g, 1.0 eq.), and the mixture kept at 80° C. for 1 h. Cooling, pouring onto crashed ice, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=9/1), delivered 4.23 g of the title compound as light brown crystals.

後処理

  1. temperatureCooling
  2. additionpouring
  3. extractionice, twofold extraction with AcOEt
  4. washwashing with water and brine
  5. dry with materialdrying over magnesium sulfate, and evaporation of the solvents

出典と根拠

ORDレコード
ord-11a5a2acbeae4b778a041cb41b2954dc
出典データセット
uspto-grants-2009_05
特許番号
US07534788B2

関連ノート

読み込み中…