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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dichloromethane → 1,3,2-Dioxathiane, 5,5-dimethyl-, 2,2-dioxide

HRID 1982583
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HRID 1982583 반응식
[CH3:1][C:2]1([CH3:9])[CH2:7][O:6][S:5](=[O:8])[O:4][CH2:3]1.C(Cl)Cl.[O-:13][Mn](=O)(=O)=O.[K+]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.O>[CH3:1][C:2]1([CH3:9])[CH2:7][O:6][S:5](=[O:13])(=[O:8])[O:4][CH2:3]1
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참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 516875Potassium PermanganateHCID 108772945,6-Dihydro-5,5-dimethyl-4H-1,3,2-dioxathiin 2-oxide

생성물 1

HCID 1205561,3,2-Dioxathiane, 5,5-dimethyl-, 2,2-dioxide수율 129.2%

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매
HCID 962
Water
용매

실험 절차

10 g (0.067 mol) of 5,5-dimethyl-1,3,2-dioxathiane 2-oxide (prepared in accordance with Example 1), 70 ml of methylene chloride, 0.76 g (0.0033 mol) of benzyltriethylammonium chloride and 70 ml of water are placed in a 350 ml four-necked flask which is provided with a stirrer and a thermometer. 7.5 g (0.0475 mol) of KMnO4 are added portion-wise at 5°-10° C. and while stirring vigorously. After the addition the reaction mixture is stirred at room temperature for a further 30 minutes and suction filtered. The organic phase is separated. The residue is washed well on the suction filter with 20 ml of methylene chloride and the aqueous phase is again extracted with this new filtrate. The combined organic phases are extracted with 1 g of NaHSO3 in 20 ml of water and washed with a small amount of water. After drying over Na2SO4 and evaporation there are obtained 10.2 g of 5,5-dimethyl-1,3,2-dioxathiane 2,2-dioxide as a white powder with a m.p. of 80°-82° C.

후처리

  1. customwhich is provided with a stirrer
  2. additionAfter the addition the reaction mixture
  3. stirringis stirred at room temperature for a further 30 minutes
  4. filtrationsuction filtered
  5. customThe organic phase is separated
  6. washThe residue is washed well on the suction
  7. filtrationfilter with 20 ml of methylene chloride
  8. extractionthe aqueous phase is again extracted with this new filtrate
  9. extractionThe combined organic phases are extracted with 1 g of NaHSO3 in 20 ml of water
  10. washwashed with a small amount of water
  11. dry with materialAfter drying over Na2SO4 and evaporation there

출처 및 근거

ORD 기록
ord-a4a55b31d87945f88cd8a8165db133d4
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04596879

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