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Dichloromethane → 1,3,2-Dioxathiane, 5,5-dimethyl-, 2,2-dioxide

HRID 1982583
ノート
印刷プレビュー

反応式

HRID 1982583 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 1205561,3,2-Dioxathiane, 5,5-dimethyl-, 2,2-dioxide収率 129.2%

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒
HCID 962
Water
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a4a55b31d87945f88cd8a8165db133d4
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04596879

反応ノート

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