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Chloride → 2-Ethylisothiazolidine 1,1-dioxide

HRID 426567
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HRID 426567 반응식
[Cl-].Cl[CH2:3][CH2:4][CH2:5][S:6]([OH:9])(=O)=[O:7].[CH2:10]([NH2:12])[CH3:11].C(O)C>C(OCC)C.C(N(CC)CC)C>[CH2:10]([N:12]1[CH2:3][CH2:4][CH2:5][S:6]1(=[O:9])=[O:7])[CH3:11]
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참가 물질

7

반응물 4

HCID 312ChlorideHCID 702EthanolHCID 6341Ethylamine2회HCID 1709623-chloropropane-1-sulfonic Acid

생성물 1

HCID 108445462-Ethylisothiazolidine 1,1-dioxide수율 70%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회
HCID 8471
Triethylamine
용매

실험 절차

To a solution of 24 g of chloride of 3-chloropropanesulfonic acid in 150 ml ethyl ether is added drop-by-drop a solution of 12 g ethylamine and 10 ml ethyl ether. The addition of the ethylamine solution is carried out under stirring and with cooling with the aid of an ice bath. After addition of the solution, the stirring is continued for 1 hour. A white precipitate of ethylamine chlorhydrate forms, which is removed by filtration upon fritted glass. Ethyl ether is removed by evaporation under reduced pressure and, to the residue obtained, is added a mixture of 4.8 g soda pellets, 400 ml ethanol and 12.5 g triethylamine. The mixture is subjected to reflux for 2 hours. After cooling, the solvent is evaporated and the residue is distilled under vacuum. There is obtained 14.2 g (yield: 70%) of N-ethylpropanesultam (boiling point under 0.1 torr: 88° C.).

후처리

  1. temperaturewith cooling with the aid of an ice bath
  2. additionAfter addition of the solution
  3. customA white precipitate of ethylamine chlorhydrate forms, which is removed by filtration upon fritted glass
  4. customEthyl ether is removed by evaporation under reduced pressure and, to the residue
  5. customobtained
  6. additionis added
  7. temperatureto reflux for 2 hours
  8. temperatureAfter cooling
  9. customthe solvent is evaporated
  10. distillationthe residue is distilled under vacuum

출처 및 근거

ORD 기록
ord-bda62fadcee9447fa355cbbe5a70495e
출처 데이터셋
uspto-grants-1979_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04170547

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