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

HRID 41810노트

반응식

HRID 41810 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 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.

후처리

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

출처 및 근거

ORD 기록
ord-bb176405ee3c4692be973994088b8f98
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08535647B2

반응 노트

불러오는 중…