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2-Chloroethyl methyl ether → HCID 554732, 화합물

HRID 1172022
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HRID 1172022 반응식
[CH3:1][O:2][CH:3]([O:14][CH3:15])[CH2:4][S:5]([CH2:8][CH:9]([O:12][CH3:13])[O:10][CH3:11])(=O)=O.COCCCl>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O>[CH3:1][O:2][CH:3]([O:14][CH3:15])[CH2:4][S:5][CH2:8][CH:9]([O:10][CH3:11])[O:12][CH3:13]
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참가 물질

5

반응물 2

HCID 123162-Chloroethyl methyl etherHCID 128158972-(2,2-Dimethoxyethanesulfonyl)-1,1-dimethoxyethane

생성물 1

HCID 554732HCID 554732, 화합물수율 63%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 962Water용매

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온도
70 °C

실험 절차

In Example 13, involving synthesis of dimethoxyethyl sulfone (DMES), 50 ml 2-chloroethyl methyl ether, 70 g Na2S.9H2O, 17.6 g tetrabutylammonium bromide and 50 ml H2O were mixed into a three-neck flask equipped with magnetic stirrer and reflux condenser, and heated at 70° C. with vigorous stirring. The reaction was continued for overnight. The organic layer was separated and dissolved in chloroform, washed with distilled water several times to remove the ammonium salt and dried over anhydrous sodium sulfate. Solvent was removed using a rotary evaporator, and dimethoxyethyl sulfide was obtained with a yield of 63%. The sulfide was oxidized with H2O2 and acetic acid, as described in Example 1, to obtain the corresponding sulfone, dimethoxyethylsulfone (DMES).

후처리

  1. additionwere mixed into a three-neck flask
  2. customequipped with magnetic stirrer
  3. temperaturereflux condenser
  4. customThe organic layer was separated
  5. dissolutiondissolved in chloroform
  6. washwashed with distilled water several times
  7. customto remove the ammonium salt
  8. dry with materialdried over anhydrous sodium sulfate
  9. customSolvent was removed
  10. customa rotary evaporator

출처 및 근거

ORD 기록
ord-797d131c3a4f47b5a6e84a9e67f5edad
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07833666B2

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