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2-Chloroethyl methyl ether → HCID 554732、化合物

HRID 1172022
ノート
印刷プレビュー

反応式

HRID 1172022 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 554732HCID 554732、化合物収率 63%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-797d131c3a4f47b5a6e84a9e67f5edad
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07833666B2

反応ノート

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