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

HRID 1915985노트

반응식

HRID 1915985 반응식
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

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 10340Sodium Carbonate2회HCID 103039Propanoic acid, 3,3-dichloro-2,2-dimethyl-HCID 23670855Potassium ethanethioate

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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. A pale yellow solid is obtained.

후처리

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

출처 및 근거

ORD 기록
ord-f96f56feecea45d791c77deec4322fcd
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08617524B2

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