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

HRID 41131ノート

反応式

HRID 41131 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 are mounted a condenser and a dropping funnel. The acid is dissolved in 80 ml of water, and 4.6 g of Na2CO3 are slowly added. 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 refluxed. After disappearance of the starting material, 7.3 ml of DMSO are added, followed by refluxing. The dithiolane is obtained after acidification by precipitating and drying the solid under vacuum.

後処理

  1. temperatureto reflux
  2. temperaturethe medium is again refluxed
  3. temperatureby refluxing

出典と根拠

ORDレコード
ord-50891be04e104c3b9b3543f1b078e9b2
出典データセット
uspto-grants-2013_09
特許番号
US08530511B2

反応ノート

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