Sodium Sulfite → 1-Bromo-4-methanesulfonyl-2-methylbenzene

HRID 422556ノート

反応式

HRID 422556 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5](SC)=[CH:4][C:3]=1[CH3:10].O[O:12][S:13]([O-:15])=O.[K+].S([O-])([O-])=O.[Na+].[Na+].[CH3:23]O.O>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:13]([CH3:23])(=[O:15])=[O:12])=[CH:4][C:3]=1[CH3:10]

参加物

5

反応物 4

HCID 24437Sodium SulfiteHCID 22242641Methanol--water (1/1)HCID 23707502Potassium hydroxy sulfiteHCID 26370189(4-Bromo-3-methylphenyl)(methyl)sulfane

生成物 1

HCID 593508361-Bromo-4-methanesulfonyl-2-methylbenzene

実験手順

To a heterogenous solution of (4-bromo-3-methylphenyl)(methyl)sulfane (2.17 g, 9.99 mmol) in 55 mL of 10/1 MeOH/water at 0° C. was added oxone (6.14 g, 9.99 mmol). The solution was allowed to warm up to RT and stirred overnight. Saturated sodium sulfite (aq.) was added and the mixture was extracted with DCM (3×). The combined organic layers were washed with water and NaCl (sat.), dried over sodium sulfate, filtered and concentrated to afford 2.30 g of 1-bromo-2-methyl-4-(methylsulfonyl)benzene 2.30 g as a white solid.

後処理

  1. extractionthe mixture was extracted with DCM (3×)
  2. washThe combined organic layers were washed with water and NaCl (sat.)
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-0de6490dabce407d8fdfb8f1625d909a
出典データセット
uspto-grants-2012_01
特許番号
US08101612B2

反応ノート

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