Methanol → Dimethyl 2,2'-dithiobisbenzoate

HRID 493098

反応式

HRID 493098 の反応式
S(=O)(=O)(O)O.[C:6]([OH:25])(=[O:24])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[S:13][S:14][C:15]1[CH:23]=[CH:22][CH:21]=[CH:20][C:16]=1[C:17]([OH:19])=O.[C:26]([O-])(O)=O.[Na+].[CH3:31][OH:32]>>[CH3:31][O:32][C:17]([C:16]1[CH:20]=[CH:21][CH:22]=[CH:23][C:15]=1[S:14][S:13][C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[C:6]([O:25][CH3:26])=[O:24])=[O:19]

参加物

5

反応物 4

HCID 887MethanolHCID 1118Sulfuric AcidHCID 8409Dithiodibenzoic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 79574Dimethyl 2,2'-dithiobisbenzoate収率 82%

実験手順

6 mL Sulphuric acid is added to ‘2,2’-dithiodibenzoic acid (20 g, 65.3 mmol) in 150 mL methanol. The reaction mixture is refluxed 3 days. The reaction mixture is cooled to room temperature and saturated aqueous NaHCO3 is added. Methanol is removed in vacuo. The resulting heterogeneous mixture is extracted with ethyl acetate. The organic phase is washed with brine, dried with MgSO4 and concentrated in vacuo to give 17.8 g (82%) of the title compound as a solid, which is used without further purification.

後処理

  1. temperatureThe reaction mixture is refluxed 3 days
  2. customMethanol is removed in vacuo
  3. extractionThe resulting heterogeneous mixture is extracted with ethyl acetate
  4. washThe organic phase is washed with brine
  5. dry with materialdried with MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-76014d977dd7498d8f65e52fe17145b8
出典データセット
uspto-grants-2009_05
特許番号
US07534791B2

関連ノート

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