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Toluene → 1-Chloro-3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)benzene

HRID 1257985
ノート
印刷プレビュー

反応式

HRID 1257985 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH3:11])(=[O:10])=[O:9])=[C:4](Cl)[C:3]=1[CH3:13].C1(C)C=CC=CC=1.[OH-].[Na+].[CH3:23][O:24][CH2:25][CH2:26][OH:27]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH3:11])(=[O:10])=[O:9])=[C:4]([O:27][CH2:26][CH2:25][O:24][CH3:23])[C:3]=1[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 1140TolueneHCID 80192-MethoxyethanolHCID 14798Sodium HydroxideHCID 672491791,3-Dichloro-2-methyl-4-(methylsulfonyl)benzene

生成物 1

HCID 668856991-Chloro-3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)benzene収率 81.2%

実験手順

1,3-Dichloro-2-methyl-4-(methylsulfonyl)benzene (13.1 g) and toluene (40 mL) were mixed, and 2-methoxyethanol (4.49 g) and sodium hydroxide (4.55 g) were added, followed by heating and refluxing for 3 hours. After completion of the reaction, the mixture was cooled to room temperature, and the solvent was distilled off under reduced pressure. To the obtained residue, a mixed solvent of methanol (12 mL) and water (48 mL) was added, followed by stirring for a while. Then, the formed solid was collected by filtration, further washed with water and dried to obtain 1-chloro-3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)benzene (12.4 g) as slightly yellow solid.

後処理

  1. temperatureby heating
  2. temperaturerefluxing for 3 hours
  3. customAfter completion of the reaction
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionTo the obtained residue, a mixed solvent of methanol (12 mL) and water (48 mL) was added
  6. filtrationThen, the formed solid was collected by filtration
  7. washfurther washed with water
  8. customdried

出典と根拠

ORDレコード
ord-a2cd616ffb7741e5906d1d36092e2778
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08466089B2

反応ノート

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