Sodium Iodide → Dimesityl disulfide

HRID 2184163

반응식

HRID 2184163 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 345613Dimesityl disulfide

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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:

후처리

  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)

출처 및 근거

ORD 기록
ord-66600d1abbe64ed2958ff894b380c2be
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900307B1

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