Sodium Iodide → Dimesityl disulfide

HRID 2184163

反応式

HRID 2184163 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[S:10](Cl)(=O)=O.[Na+].[I-].FCC(O[C:21](=O)[CH2:22]F)=O>CC(C)=O>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[S:10][S:10][C:3]1[C:2]([CH3:1])=[CH:7][C:6]([CH3:8])=[CH:5][C:21]=1[CH3:22]

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 130462-Mesitylenesulfonyl chlorideHCID 67886Acetic acid, 2-fluoro-, 1,1'-anhydride

生成物 1

HCID 345613Dimesityl disulfide

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

2,4,6-trimethylphenylsulfonyl chloride (500 mg, 2.3 mmol) was dissolved in acetone (60 mL), and then NaI (3.4 g, 23 mmol) and fluoroacetic anhydride (1.45 mL, 6.9 mmol) were added and the mixture was stirred at room temperature for one hour. The reaction solution was concentrated, water was added, extraction was performed with ether and the organic layer was further washed with aqueous sodium thiosulfate, water and saturated saline. After drying over magnesium sulfate and vacuum concentration, the residue was purified with a silica gel column (hexane) to obtain 2,4,6-trimethylphenyldisulfide as a light yellow crystalline compound (231 mg, 0.76 mmol, 67% yield). The NMR and mass spectral data for the obtained compound were as follows:

後処理

  1. concentrationThe reaction solution was concentrated
  2. additionwater was added
  3. extractionextraction
  4. washthe organic layer was further washed with aqueous sodium thiosulfate, water and saturated saline
  5. dry with materialAfter drying over magnesium sulfate and vacuum concentration
  6. customthe residue was purified with a silica gel column (hexane)

出典と根拠

ORDレコード
ord-66600d1abbe64ed2958ff894b380c2be
出典データセット
uspto-grants-2005_05
特許番号
US06900307B1

関連ノート

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