Dimethyl Sulfoxide → 4-Methyl-1,2-dithiolane-4-carboxylic acid

HRID 41810ノート

反応式

HRID 41810 の反応式
Cl[CH:2](Cl)[C:3]([CH3:8])(C)[C:4]([OH:6])=[O:5].C([O-])([O-])=O.[Na+].[Na+].C([O-])(=[S:18])C.[K+].C[S:22]([CH3:24])=O>O>[CH3:8][C:3]1([C:4]([OH:6])=[O:5])[CH2:24][S:22][S:18][CH2:2]1

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 10340Sodium Carbonate2 回HCID 103039Propanoic acid, 3,3-dichloro-2,2-dimethyl-HCID 23670855Potassium ethanethioate

生成物 1

HCID 200693114-Methyl-1,2-dithiolane-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

8 g of dichloropivalic acid are placed in a 250 ml three-necked flask on which is mounted a condenser and a dropping funnel. The acid is dissolved in 80 ml of water, slowly adding 4.6 g of Na2CO3. A solution of 10.7 g of potassium thioacetate is added dropwise and the reaction medium is brought to reflux. 14.9 g of Na2CO3 are added and the medium is again heated at reflux. After disappearance of the starting material, 7.3 ml of DMSO are added, followed by refluxing. The dithiolane is obtained after acidification by precipitation and drying of the solid under vacuum. A pale yellow solid is obtained.

後処理

  1. temperatureto reflux
  2. temperaturethe medium is again heated
  3. temperatureat reflux
  4. temperatureby refluxing

出典と根拠

ORDレコード
ord-bb176405ee3c4692be973994088b8f98
出典データセット
uspto-grants-2013_09
特許番号
US08535647B2

反応ノート

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